CN103824959A - Ink for forming functional layer, ink container, discharging apparatus, method for forming functional layer, method for manufacturing organic EL element, light emitting device, and electronic apparatus - Google Patents
Ink for forming functional layer, ink container, discharging apparatus, method for forming functional layer, method for manufacturing organic EL element, light emitting device, and electronic apparatus Download PDFInfo
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- CN103824959A CN103824959A CN201310566536.5A CN201310566536A CN103824959A CN 103824959 A CN103824959 A CN 103824959A CN 201310566536 A CN201310566536 A CN 201310566536A CN 103824959 A CN103824959 A CN 103824959A
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- 238000000034 method Methods 0.000 title claims abstract description 99
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 238000007599 discharging Methods 0.000 title abstract 2
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- 238000009835 boiling Methods 0.000 claims abstract description 412
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- FUGIIBWTNARRSF-UHFFFAOYSA-N decane-5,6-diol Chemical compound CCCCC(O)C(O)CCCC FUGIIBWTNARRSF-UHFFFAOYSA-N 0.000 claims description 24
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- HYLLZXPMJRMUHH-UHFFFAOYSA-N 1-[2-(2-methoxyethoxy)ethoxy]butane Chemical compound CCCCOCCOCCOC HYLLZXPMJRMUHH-UHFFFAOYSA-N 0.000 claims description 21
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- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 4
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- ZBZXYUYUUDZCNB-UHFFFAOYSA-N N-cyclohexa-1,3-dien-1-yl-N-phenyl-4-[4-(N-[4-[4-(N-[4-[4-(N-phenylanilino)phenyl]phenyl]anilino)phenyl]phenyl]anilino)phenyl]aniline Chemical compound C1=CCCC(N(C=2C=CC=CC=2)C=2C=CC(=CC=2)C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C=CC(=CC=2)C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C=CC(=CC=2)C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 ZBZXYUYUUDZCNB-UHFFFAOYSA-N 0.000 description 1
- 229930192627 Naphthoquinone Chemical class 0.000 description 1
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 1
- NRCMAYZCPIVABH-UHFFFAOYSA-N Quinacridone Chemical compound N1C2=CC=CC=C2C(=O)C2=C1C=C1C(=O)C3=CC=CC=C3NC1=C2 NRCMAYZCPIVABH-UHFFFAOYSA-N 0.000 description 1
- 101100457453 Saccharomyces cerevisiae (strain ATCC 204508 / S288c) MNL1 gene Proteins 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 1
- 102100029887 Translationally-controlled tumor protein Human genes 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- GWFGARXUJNKOMY-UHFFFAOYSA-N [3,5-di(carbazol-9-yl)phenyl]-triphenylsilane Chemical compound C1=CC=CC=C1[Si](C=1C=C(C=C(C=1)N1C2=CC=CC=C2C2=CC=CC=C21)N1C2=CC=CC=C2C2=CC=CC=C21)(C=1C=CC=CC=1)C1=CC=CC=C1 GWFGARXUJNKOMY-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- HAQFCILFQVZOJC-UHFFFAOYSA-N anthracene-9,10-dione;methane Chemical class C.C.C1=CC=C2C(=O)C3=CC=CC=C3C(=O)C2=C1 HAQFCILFQVZOJC-UHFFFAOYSA-N 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002772 conduction electron Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- VBVAVBCYMYWNOU-UHFFFAOYSA-N coumarin 6 Chemical compound C1=CC=C2SC(C3=CC4=CC=C(C=C4OC3=O)N(CC)CC)=NC2=C1 VBVAVBCYMYWNOU-UHFFFAOYSA-N 0.000 description 1
- 150000001934 cyclohexanes Chemical class 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- OPTDDWCXQQYKGU-UHFFFAOYSA-N diphenyldichloromethane Chemical compound C=1C=CC=CC=1C(Cl)(Cl)C1=CC=CC=C1 OPTDDWCXQQYKGU-UHFFFAOYSA-N 0.000 description 1
- CZZYITDELCSZES-UHFFFAOYSA-N diphenylmethane Chemical compound C=1C=CC=CC=1CC1=CC=CC=C1 CZZYITDELCSZES-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229920001179 medium density polyethylene Polymers 0.000 description 1
- 239000004701 medium-density polyethylene Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- CELAVSIYCCQNGG-UHFFFAOYSA-N n-(4-cyclohexylphenyl)-4-methyl-n-(4-methylphenyl)aniline Chemical class C1=CC(C)=CC=C1N(C=1C=CC(=CC=1)C1CCCCC1)C1=CC=C(C)C=C1 CELAVSIYCCQNGG-UHFFFAOYSA-N 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 150000002791 naphthoquinones Chemical class 0.000 description 1
- VOFUROIFQGPCGE-UHFFFAOYSA-N nile red Chemical compound C1=CC=C2C3=NC4=CC=C(N(CC)CC)C=C4OC3=CC(=O)C2=C1 VOFUROIFQGPCGE-UHFFFAOYSA-N 0.000 description 1
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N o-biphenylenemethane Natural products C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 description 1
- 150000004866 oxadiazoles Chemical class 0.000 description 1
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- JZRYQZJSTWVBBD-UHFFFAOYSA-N pentaporphyrin i Chemical compound N1C(C=C2NC(=CC3=NC(=C4)C=C3)C=C2)=CC=C1C=C1C=CC4=N1 JZRYQZJSTWVBBD-UHFFFAOYSA-N 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 description 1
- CSHWQDPOILHKBI-UHFFFAOYSA-N peryrene Natural products C1=CC(C2=CC=CC=3C2=C2C=CC=3)=C3C2=CC=CC3=C1 CSHWQDPOILHKBI-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- HRGDZIGMBDGFTC-UHFFFAOYSA-N platinum(2+) Chemical compound [Pt+2] HRGDZIGMBDGFTC-UHFFFAOYSA-N 0.000 description 1
- HWLDNSXPUQTBOD-UHFFFAOYSA-N platinum-iridium alloy Chemical class [Ir].[Pt] HWLDNSXPUQTBOD-UHFFFAOYSA-N 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- 150000004059 quinone derivatives Chemical class 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- YYMBJDOZVAITBP-UHFFFAOYSA-N rubrene Chemical compound C1=CC=CC=C1C(C1=C(C=2C=CC=CC=2)C2=CC=CC=C2C(C=2C=CC=CC=2)=C11)=C(C=CC=C2)C2=C1C1=CC=CC=C1 YYMBJDOZVAITBP-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 125000005504 styryl group Chemical group 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- JLAVCPKULITDHO-UHFFFAOYSA-N tetraphenylsilane Chemical compound C1=CC=CC=C1[Si](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 JLAVCPKULITDHO-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000010023 transfer printing Methods 0.000 description 1
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical compound [Al+3].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 TVIVIEFSHFOWTE-UHFFFAOYSA-K 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- 125000006617 triphenylamine group Chemical class 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/36—Inkjet printing inks based on non-aqueous solvents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
- H10K71/135—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing using ink-jet printing
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
- H10K50/12—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising dopants
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/16—Electron transporting layers
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
Abstract
The present invention provides an ink for forming a functional layer suitable for forming a functional layer by using a liquid phase technology (ink-jet method), an ink container, a discharging apparatus, a method for forming the functional layer, a method for manufacturing an organic EL element, a light emitting device, and an electronic apparatus. The ink for forming the functional layer includes a first component that contains at least one kind of aromatic solvent of which a boiling point is higher than or equal to 250 DEG C and lower than or equal to 350 DEG C, a second component that contains at least one kind of aliphatic solvent of which a boiling point is higher than or equal to 200 DEG C, and a third component that is a positive hole injection material (m-MTDATA) for forming a positive hole injection layer, in which a solubility of the third component in the first component is higher than the solubility of the third component in the second component, a mixing ratio of the second component is 30 vol%, the boiling point of the first component is higher than the boiling point of the second component, and a difference between the boiling points thereof is higher than or equal to 30 DEG C.
Description
Technical field
The present invention relates to functional layer forms with ink, ink reservoir, blowoff, the formation method of functional membrane, manufacture method, light-emitting device, the electronic equipment of organic electroluminescent (EL) element.
Background technology
In recent years, as the method for the functional layer such as the semi-conductive electrode such as luminescent layer, OTFT, semiconductor layer of dyed layer (filter course), organic EL that forms colour filter, developed the method that uses liquid phase process.In liquid phase process, ink-jet method (being also referred to as drop ejection method) is as the ink of ormal weight (solution) being coated on to the method for desirable position well and getting most of the attention from shower nozzle (ink-spraying-head) precision with the form of drop.
On the other hand, the ink (solution) using in ink-jet method, once cause solid constituent to be separated out at the nozzle of shower nozzle because of dry, can cause the obstruction of nozzle, the landing positions of drop occurs at random or bad from inconsistent etc. the ejection of the spray volume of the drop of nozzle ejection.Therefore, seek a kind of difficult generation and spray bad ink (solution).In addition, because be is dried to form functional layer (functional membrane) after ink (solution) is coated with, so requirement can be coated with in desirable region equably to applied things such as substrates.
For example, in patent documentation 1, a kind of amorphous film formation ink composite is disclosed, its solubility that contains organic material is more than 0.5wt% the 1st solvent and is the 2nd solvent that 0.1wt% is following and 120 ℃ of above alcoholic compounds of boiling point form by the solubility of organic material, and the boiling point of the 1st solvent is higher than the boiling point of the 2nd solvent.Record according to patent documentation 1, this amorphous film formation is suitable for ink-jet method with ink composite.
In addition, for example, in patent documentation 2, a kind of coating fluid is disclosed, be the coating fluid that contains mixed solvent and functional material, mixed solvent contains the 1st solvent and other solvent, and described the 1st solvent is made up of the compound that has 2 above aromatic rings and have a symmetrical structure.If use this coating fluid, in ink-jet method, be difficult for causing the obstruction of nozzle, can realize stable ejection.
In addition, for example, in patent documentation 3, a kind of solutions of organic semiconductors is disclosed, it contains at least a kind of organic solvent A as organic semi-conductor good solvent and at least a kind of organic solvent B as organic semi-conductor poor solvent, and the boiling point of organic solvent A is higher than the boiling point of organic solvent B.Utilize this solution, when dry, the difficult cohesion of organic semiconducting materials is separated out, and can carry out the film forming of homogeneous, can form the organic semiconductor with stable electrical characteristics.
Prior art document
Patent documentation
Patent documentation 1: No. 4616596 communique of Japan Patent
Patent documentation 2: No. 4707658 communique of Japan Patent
Patent documentation 3: No. 5019454 communique of Japan Patent
Summary of the invention
But, for the ink composite of above-mentioned patent documentation 1, because the 2nd solvent is alcoholic compound, so there is the easily such problem of cohesion of organic material in the dry run of the ink composite being coated with.In addition, for the coating fluid of patent documentation 2, because the solvent of the first solvent and other is aromatic compound, so coating fluid is ejected into drop form on the conducting film of metal, metal oxide etc. if had, be difficult to wetting expansion, easily produce the problem of crawling.In addition, for the solutions of organic semiconductors of patent documentation 3, organic solvent B in this solution the preferred ratio lower than organic solvent A due to boiling point is below 30 volume %, so in the drying process of this solution being coated with, compared with organic solvent A, the time that organic solvent B is first evaporated early.Therefore,, if the remaining organic solvent A as good solvent is poor to the wetability of applied thing after organic solvent B evaporation, easily produce the problem of crawling.In other words,, for the solution shown in patent documentation 1～patent documentation 3 forms, there is the problem that possibly cannot be formed uniformly functional layer (functional membrane).
The present invention carries out at least a portion that solves above-mentioned problem, can realize by following mode or application examples.
Application examples 1
The functional layer formation ink should use-case relating to, it is characterized in that, the 1st composition that at least a kind of aromatic solvent that to contain by boiling point be 250 ℃～350 ℃ forms, be 200 ℃ of the 2nd compositions that at least a kind of above aliphatic solvent forms by boiling point, the 3rd composition with functional layer formation use, for the dissolubility of above-mentioned the 3rd composition, be that above-mentioned the 1st composition is higher than above-mentioned the 2nd composition, the mixing ratio of above-mentioned the 2nd composition is 30 volume %～70 volume %, the boiling point of above-mentioned the 1st composition is higher than the boiling point of above-mentioned the 2nd composition, the difference of the boiling point of the boiling point of above-mentioned the 1st composition and above-mentioned the 2nd composition is more than 30 ℃.
According to should use-case, because combination aromatic solvent and aliphatic solvent form the mixed solvent for the 3rd composition, so compared with the situation independent with aromatic solvent, easily adjust dissolubility and the surface tension to the 3rd composition.In addition, because the boiling point of the 2nd composition (aliphatic solvent) compared with dissolving the 1st composition (aromatic solvent) of the 3rd composition is low, and be more than 200 ℃, so be difficult for producing the obstruction due to nozzle dry of shower nozzle.In addition, because the 2nd composition is aliphatic solvent, so even if conducting film is also shown to excellent wetability, be difficult for producing crawling.In addition, the difference of the boiling point of the boiling point of the 1st composition and the 2nd composition is more than 30 ℃, and the 2nd composition is 30 volume %～70 volume % in the shared mixing ratio of ink entirety.Therefore, lower than compared with the situation of 30 volume %, avoid the 2nd composition in drying process to evaporate rapidly with the 2nd composition, be difficult for producing the caused crawling of rate of drying of the 2nd composition., can provide one to be suitable for the functional layer formation ink of ink-jet method (drop ejection method).
Application examples 2
The functional layer that above-mentioned application examples relates to forms with in ink, it is characterized in that, above-mentioned the 2nd composition is less than above-mentioned the 1st component list surface tension, and the surface tension of above-mentioned the 2nd composition is below 32mN/m.
According to this point, can provide applied thing is shown to excellent wetability, be more difficult to produce the functional layer formation ink of crawling.
Application examples 3
The functional layer that above-mentioned application examples relates to forms with in ink, it is characterized in that, the n that above-mentioned the 2nd composition is following chemical formulation is more than 2 aliphat ethers.
RO-(CH
2o)
n-R (R is alkyl).
Application examples 4
The functional layer that above-mentioned application examples relates to forms with in ink, it is characterized in that, above-mentioned the 2nd composition is selected from diethylene glycol butyl methyl ether or dibutyl ethylene glycol ether.
According to this point, can obtain and surface tension little with the aromatic solvent phase specific surface tension of the 1st composition is the 2nd composition below 32mN/m.
Application examples 5
Functional layer that above-mentioned application examples relates to forms with in ink, it is characterized in that, above-mentioned the 1st composition is any the aromatic compound in, oxygen nitrogenous at side chain, fluorine, chlorine.
Application examples 6
The functional layer that above-mentioned application examples relates to forms with in ink, it is characterized in that, above-mentioned the 1st composition is selected from benzyl ether, 3-phenoxytoluene, 1, two (3, the 4-3,5-dimethylphenyl) ethane of 1-.
The boiling point of these aromatic solvents is more than 250 ℃, and organic semiconducting materials is shown to excellent dissolubility.
Application examples 7
The functional layer relating in above-mentioned application examples forms with in ink, and preferably above-mentioned the 1st composition dissolves above-mentioned the 3rd composition more than 0.1wt%.
Application examples 8
The functional layer relating in above-mentioned application examples forms with in ink, and the mixed solvent of above-mentioned the 1st composition and above-mentioned the 2nd composition can dissolve above-mentioned the 3rd composition more than 0.1wt%.
According to these application examples, even if the thinner functional layer of thickness also can be used ink-jet method stably to form.
Application examples 9
The functional layer that above-mentioned application examples relates to forms with in ink, it is characterized in that, above-mentioned the 1st composition contains multiple aromatic solvent.
According to this point, and be compared with a kind of aromatic solvent, easily adjust the dissolubility of the 3rd composition, wetability to applied thing etc.
Application examples 10
The functional layer that above-mentioned application examples relates to forms with in ink, it is characterized in that, above-mentioned the 3rd composition contains as containing pi-conjugated macromolecular material or the organic compound containing pi-conjugated low molecular material.
If use this functional layer to form ink, can without crawling form the functional layer being formed by organic compound.Should illustrate, low molecular material refers to the material that molecular weight is less than 1000.In addition, macromolecular material refers to that molecular weight is more than 1000 and has the material of structure that basic framework repeats.
Application examples 11
The functional layer that above-mentioned application examples relates to forms with in ink, it is characterized in that, above-mentioned the 3rd composition further contains metal complex.
If use this functional layer to form ink, for example can without crawling form the luminescent layer as the functional layer take metal complex as luminescent material, take organic compound as material of main part.
Application examples 12
The functional layer that above-mentioned application examples relates to forms with in ink, it is characterized in that, above-mentioned the 3rd composition contains multiple organic compound.
If use this functional layer to form ink, can without crawling form the functional layer that contains multiple organic compound.
Application examples 13
The ink reservoir should use-case relating to, is characterized in that, the functional layer formation ink of recording in above-mentioned application examples is inside housed.
Application examples 14
The blowoff should use-case relating to, it is characterized in that, possess the ink reservoir of recording in above-mentioned application examples and the shower nozzle of supplying with above-mentioned functions layer formation ink from above-mentioned ink reservoir, above-mentioned shower nozzle sprays the formation of above-mentioned functions layer with drop form with ink from nozzle.
According to should use-case, can provide the blowoff that utilizes ink-jet method (drop ejection method) can form the functional layer that crawling is few.
Application examples 15
The formation method of the functional layer should use-case relating to, it is characterized in that, possess the functional layer of recording in above-mentioned application examples is formed to the operation that is coated on the film formation region of applied thing with ink, solidify with ink setting with the above-mentioned functions layer being coated with is formed, form region and form the operation of functional layer at above-mentioned film.
According to should use-case, can provide the functional layer formation method that can utilize liquid phase process to form the functional layer that crawling is few.
Application examples 16
In the functional layer formation method of above-mentioned application examples, preferred above-mentioned film formation region is separated with the next door that ink is had liquid repellency the formation of above-mentioned functions layer.
According to the method, functional layer formation is filled in equably with ink the film being separated into by next door and is formed region.
Application examples 17
The manufacture method of the organic EL should use-case relating to, it is characterized in that, be the manufacture method having between anode and negative electrode containing the organic EL of the functional layer of luminescent layer, possess following operation: form the operation of separating the insulating barrier of above-mentioned anode according to the mode overlapping with the outer rim of above-mentioned anode and form peristome on above-mentioned anode; Be coated with at above-mentioned peristome the functional layer of recording in above-mentioned application examples and form the operation with ink; The above-mentioned functions layer being coated with is formed and solidified with ink setting, form the operation of at least 1 layer in above-mentioned functions layer; And cover above-mentioned insulating barrier and above-mentioned functions layer and form the operation of above-mentioned negative electrode.
According to should use-case, form with the few state of crawling due at least 1 layer in functional layer, so can rate of finished products manufacture well the organic EL with the desirable characteristics of luminescence.
Application examples 18
The light-emitting device should use-case relating to, is characterized in that, possesses the organic EL that utilizes the manufacture method of the organic EL of recording in above-mentioned application examples to manufacture.
According to should use-case, can provide and possess light-emitting device organic EL, that realized excellent display quality with the desirable characteristics of luminescence.
Application examples 19
The electronic equipment should use-case relating to, is characterized in that possessing the light-emitting device of recording in above-mentioned application examples.
According to should use-case, can provide the electronic equipment with excellent display quality.
Accompanying drawing explanation
Fig. 1 is the concise and to the point vertical view that represents the formation of light-emitting device.
Fig. 2 is the schematic section that represents the formation of organic EL.
Fig. 3 is the sketch that represents the formation of blowoff.
Fig. 4 is the concise and to the point stereogram that represents the formation of shower nozzle.
In Fig. 5, (a) is the stereogram representing as the print cartridge of ink reservoir, is (b) sectional view that represents the structure of print cartridge.
(a) in Fig. 6～(d) is the fragmentary cross sectional view that represents the manufacture method of organic EL.
Fig. 7 represents that hole injection layer forms the formation of the comparative example 1-1～comparative example 1-25 that uses ink and the table of evaluation result.
Fig. 8 represents that hole injection layer forms the formation of the comparative example 1-26～comparative example 1-50 that uses ink and the table of evaluation result.
Fig. 9 represents that hole injection layer forms the formation of the comparative example 1-51～comparative example 1-75 that uses ink and the table of evaluation result.
Figure 10 represents that hole injection layer forms the formation of the comparative example 1-76～comparative example 1-100 that uses ink and the table of evaluation result.
Figure 11 represents that hole injection layer forms the formation of the embodiment 1-1～embodiment 1-25 that uses ink and the table of evaluation result.
Figure 12 represents that hole injection layer forms comparative example 1-101～comparative example 1-116 and the formation of embodiment 1-26～embodiment 1-34 and the table of evaluation result with ink.
Figure 13 represents that hole injection layer forms comparative example 1-117～comparative example 1-137 and the formation of embodiment 1-35～embodiment 1-38 and the table of evaluation result with ink.
Figure 14 represents that hole injection layer forms the formation of the embodiment 1-39～embodiment 1-63 that uses ink and the table of evaluation result.
Figure 15 represents that hole injection layer forms comparative example 1-138～comparative example 1-153 and the formation of embodiment 1-64～embodiment 1-72 and the table of evaluation result with ink.
Figure 16 represents that hole injection layer forms comparative example 1-154～comparative example 1-174 and the formation of embodiment 1-73～embodiment 1-76 and the table of evaluation result with ink.
Figure 17 represents that hole injection layer forms the formation of the embodiment 1-77～embodiment 1-101 that uses ink and the table of evaluation result.
Figure 18 is that hole injection layer forms comparative example 1-175～comparative example 1-190 and the formation of embodiment 1-102～embodiment 1-110 and the table of evaluation result with ink.
Figure 19 represents that hole injection layer forms comparative example 1-191～comparative example 1-211 and the formation of embodiment 1-111～embodiment 1-114 and the table of evaluation result with ink.
Figure 20 represents that hole injection layer forms the formation of the comparative example 1-212～comparative example 1-236 that uses ink and the table of evaluation result.
Figure 21 represents that hole injection layer forms the formation of the comparative example 1-237～comparative example 1-261 that uses ink and the table of evaluation result.
Figure 22 represents that hole injection layer forms the formation of the comparative example 1-262～comparative example 1-286 that uses ink and the table of evaluation result.
Figure 23 represents that hole transporting layer forms the formation of the comparative example 2-1～comparative example 2-25 that uses ink and the table of evaluation result.
Figure 24 represents that hole transporting layer forms the formation of the comparative example 2-26～comparative example 2-50 that uses ink and the table of evaluation result.
Figure 25 represents that hole transporting layer forms the formation of the comparative example 2-51～comparative example 2-75 that uses ink and the table of evaluation result.
Figure 26 represents that hole transporting layer forms the formation of the comparative example 2-76～comparative example 2-100 that uses ink and the table of evaluation result.
Figure 27 represents that hole transporting layer forms the formation of the embodiment 2-1～embodiment 2-25 that uses ink and the table of evaluation result.
Figure 28 represents that hole transporting layer forms comparative example 2-101～comparative example 2-116 and the formation of embodiment 2-26～embodiment 2-34 and the table of evaluation result with ink.
Figure 29 represents that hole transporting layer forms comparative example 2-117～comparative example 2-137 and the formation of embodiment 2-35～embodiment 2-38 and the table of evaluation result with ink.
Figure 30 represents that hole transporting layer forms the formation of the embodiment 2-39～embodiment 2-63 that uses ink and the table of evaluation result.
Figure 31 represents that hole transporting layer forms comparative example 2-138～comparative example 2-153 and the formation of embodiment 2-64～embodiment 2-72 and the table of evaluation result with ink.
Figure 32 represents that hole transporting layer forms comparative example 2-154～comparative example 2-174 and the formation of embodiment 2-73～embodiment 2-76 and the table of evaluation result with ink.
Figure 33 represents that hole transporting layer forms the formation of the embodiment 2-77～embodiment 2-101 that uses ink and the table of evaluation result.
Figure 34 represents that hole transporting layer forms comparative example 2-175～comparative example 2-190 and the formation of embodiment 2-102～embodiment 2-110 and the table of evaluation result with ink.
Figure 35 represents that hole transporting layer forms comparative example 2-191～comparative example 2-211 and the formation of embodiment 2-111～embodiment 2-114 and the table of evaluation result with ink.
Figure 36 represents that hole transporting layer forms the formation of the comparative example 2-212～comparative example 2-236 that uses ink and the table of evaluation result.
Figure 37 represents that hole transporting layer forms the formation of the comparative example 2-237～comparative example 2-261 that uses ink and the table of evaluation result.
Figure 38 represents that hole transporting layer forms the formation of the comparative example 2-262～comparative example 2-286 that uses ink and the table of evaluation result.
Figure 39 represents that luminescent layer forms the formation of the comparative example 3-1～comparative example 3-25 that uses ink and the table of evaluation result.
Figure 40 represents that luminescent layer forms the formation of the comparative example 3-26～comparative example 3-50 that uses ink and the table of evaluation result.
Figure 41 represents that luminescent layer forms the formation of the comparative example 3-51～comparative example 3-75 that uses ink and the table of evaluation result.
Figure 42 represents that luminescent layer forms the formation of the comparative example 3-76～comparative example 3-100 that uses ink and the table of evaluation result.
Figure 43 represents that luminescent layer forms the formation of the embodiment 3-1～embodiment 3-25 that uses ink and the table of evaluation result.
Figure 44 represents that luminescent layer forms comparative example 3-101～comparative example 3-116 and the formation of embodiment 3-26～embodiment 3-34 and the table of evaluation result with ink.
Figure 45 represents that luminescent layer forms comparative example 3-117～comparative example 3-137 and the formation of embodiment 3-35～embodiment 3-38 and the table of evaluation result with ink.
Figure 46 represents that luminescent layer forms the formation of the embodiment 3-39～embodiment 3-63 that uses ink and the table of evaluation result.
Figure 47 is that luminescent layer forms comparative example 3-138～comparative example 3-153 and the formation of embodiment 3-64～embodiment 3-72 and the table of evaluation result with ink.
Figure 48 represents that luminescent layer forms comparative example 3-154～comparative example 3-174 and the formation of embodiment 3-73～embodiment 3-76 and the table of evaluation result with ink.
Figure 49 represents that luminescent layer forms the formation of the embodiment 3-77～embodiment 3-101 that uses ink and the table of evaluation result.
Figure 50 represents that luminescent layer forms comparative example 3-175～comparative example 3-190 and the formation of embodiment 3-102～embodiment 3-110 and the table of evaluation result with ink.
Figure 51 represents that luminescent layer forms comparative example 3-191～comparative example 3-211 and the formation of embodiment 3-111～embodiment 3-114 and the table of evaluation result with ink.
Figure 52 represents that luminescent layer forms the formation of the comparative example 3-212～comparative example 3-236 that uses ink and the table of evaluation result.
Figure 53 represents that luminescent layer forms the formation of the comparative example 3-237～comparative example 3-261 that uses ink and the table of evaluation result.
Figure 54 represents that luminescent layer forms the formation of the comparative example 3-262～comparative example 3-286 that uses ink and the table of evaluation result.
In Figure 55, (a) is the sketch representing as the notebook computer of an example of electronic equipment, is (b) sketch as the panel TV (TV) of an example of electronic equipment.
Embodiment
Below, with reference to the accompanying drawings to execution mode specific the present invention is described.Should illustrate, for the part that makes explanation becomes discernible state, the accompanying drawing of use is suitably zoomed in or out to represent.
The 1st execution mode
Light-emitting device
First, see figures.1.and.2 the light-emitting device of present embodiment is described.Fig. 1 is the concise and to the point vertical view that represents the formation of light-emitting device, and Fig. 2 is the schematic section that represents the formation of organic EL.
As shown in Figure 1, the light-emitting device 100 of present embodiment has device substrate 101, and this device substrate 101 disposes sub-pixel 110R, 110G, the 110B that can obtain redness (R), green (G), blue (B) luminous (illuminant colour).Each sub-pixel 110R, 110G, 110B are roughly rectangle, in the E of the viewing area of device substrate 101, are rectangular configuration.Below, also sub-pixel 110R, 110G, 110B are commonly referred to as to sub-pixel 110.The sub-pixel 110 of identical illuminant colour on figure vertically (row to or the long side direction of sub-pixel 110) arrange, the sub-pixel 110 of different illuminant colours along continuous straight runs (row to or the short side direction of sub-pixel 110) on figure is arranged with the order of R, G, B., sub-pixel 110R, the 110G of different illuminant colours, 110B configure in so-called striped mode.Should illustrate, flat shape and the configuration of sub-pixel 110R, 110G, 110B are not limited to this.In addition, essentially rectangular, except square, rectangle, also comprises that it is circular-arc quadrangle that bight becomes round quadrangle, opposed 2 limit portions.
At sub-pixel 110R, be provided with and can obtain the luminous organic electroluminescent as light-emitting component of redness (R) (EL) element.Similarly, at sub-pixel 110G, be provided with and can obtain the luminous organic EL as light-emitting component of green (G), at sub-pixel 110B, be provided with and can obtain the luminous organic EL as light-emitting component of blueness (B).
Such light-emitting device 100 is subject to electric control take 3 sub-pixel 110R, the 110G, the 110B that obtain different illuminant colours as 1 display pixel unit, each sub-pixel 110R, 110G, 110B.Can become thus full color shows.
At each sub-pixel 110R, 110G, 110B, be provided with the organic EL 130 as light-emitting component shown in Fig. 2.
Functional layer 136 has stacked gradually hole injection layer 131, hole transporting layer 132, luminescent layer 133, electron supplying layer 134, electron injecting layer 135 from pixel electrode 102 sides.Especially luminescent layer 133 is selected constituent material according to illuminant colour, but is which kind of is all referred to as luminescent layer 133 at this illuminant colour.Should illustrate, the formation of functional layer 136 is not limited to this, except these layers, can also possess the intermediate layer of the movement of control charge carrier (hole, electronics) etc.
Opposite electrode 103 is as negative electrode performance function, arranges as sub-pixel 110R, 110G, the shared common electrode of 110B, for example, uses the formation such as alloy of Al (aluminium) or Ag (silver) and Mg (magnesium).
Inject the hole as charge carrier from the pixel electrode 102 lateral direction light emission layers 133 as anode, inject the electronics as charge carrier from the opposite electrode 103 lateral direction light emission layers 133 as negative electrode.In luminescent layer 133, utilize the hole and the electronics that are injected into, form exciton (exciton; The state that hole and electronics fetter mutually because of Coulomb force), when exciton (exciton) disappears, the part of (hole and electronics again in conjunction with time) energy becomes fluorescence, phosphorescence is released.
In light-emitting device 100, if form opposite electrode 103 for example to there is the mode of reflective, because pixel electrode 102 has light transmission, so can make to penetrate from device substrate 101 sides from the light of luminescent layer 133.Such illumination mode is called as bottom emission mode.In addition, if reflector is set between device substrate 101 and pixel electrode 102, form opposite electrode 103 to there is the mode of light transmission, also can become the top emission design penetrating from opposite electrode 103 sides from the light of luminescent layer 133.In the present embodiment, light-emitting device 100, as bottom emission mode, carries out the following description.
In the present embodiment, light-emitting device 100 has the next door 104 as the insulating barrier in the present invention, the outer rim of the pixel electrode 102 in the organic EL 130 of this next door 104 and each sub-pixel 110R, 110G, 110B overlaps, and forms peristome 104a on pixel electrode 102.
In the present embodiment, for the functional layer 136 of organic EL 130, at least 1 layer in the hole injection layer 131 of formation functional layer 136, hole transporting layer 132, luminescent layer 133 forms with liquid phase process.Liquid phase process refers to the solution (hereinafter referred to as functional layer formation ink) of the 3rd composition that contains each layer of formation and solvent thereby being coated on to form the peristome 104a in region and it is dried as the film being impaled by next door 104 forms the method for each layer.In order to form each layer with desirable thickness, the functional layer formation of ormal weight need to be coated on to peristome 104a well by ink precision, in the present embodiment, adopt ink-jet method (also referred to as drop ejection method) as liquid phase process.
Blowoff
Next, with reference to Fig. 3～Fig. 5 to the specific blowoff of ink-jet method (drop ejection method) is described.Fig. 3 is the sketch that represents the formation of blowoff, and Fig. 4 is the concise and to the point stereogram that represents the formation of shower nozzle, and Fig. 5 (a) is the stereogram representing as the print cartridge of ink reservoir, and Fig. 5 (b) is the sectional view that represents the structure of print cartridge.
As shown in Figure 3, the blowoff 1 of present embodiment possesses: as be placed with target be substrate W mounting table objective table 7 and functional layer is formed and sprays to the shower nozzle 20 of the substrate W of mounting with ink with drop form.In addition, possess inking mechanism, it is supplied with by pipe arrangement 13 functional layer formation from the memory function layer formation ink tank 14 of ink with ink to shower nozzle 20.
In addition, blowoff 1 possesses the cleaning mechanism 8 for clean (Recovery processing) shower nozzle 20.In cleaning mechanism 8, also possesses Y-axis drive motors 6 in addition.
At head cartridge 10, with nozzle face 28a (with reference to Fig. 4) and the opposed mode mounting spray head 20 of objective table 7.The functional layer that the ejection voltage of shower nozzle 20 based on being supplied with by control part 15 can make to be ejected forms by the amount (hereinafter referred to as spray volume) of the drop of ink variable.
Same Y- axis drive motors 5,6 is not limited to this, for example, be stepping motor etc., while supplying with the drive pulse signal of Y-direction, the Y-direction axis of guide 4 is rotated from control part 15, and objective table 7 and cleaning mechanism 8 are moved in Y-direction.
As shown in Figure 4, shower nozzle 20 is so-called 2 row's shower nozzles, possesses: the functional layer with 2 rows' connecting needle 24 forms by the introduction part 23 of ink, is layered in the printhead substrate 25 of introduction part 23 and is configured on printhead substrate 25 and the inner functional layer that is formed with forms the nozzle body 26 with the interior stream of shower nozzle of ink.Connecting needle 24 is situated between and is connected with above-mentioned ink tank 14 by pipe arrangement 13, is situated between and is formed and be fed into stream in shower nozzle with ink by connecting needle 24 functional layers.Be provided with 2 connectors 29 of arranging that are situated between and are connected with shower nozzle drive division by flexible flat cable at printhead substrate 25.
For 2 nozzle rows 22,22, multiple (180) nozzle 21 is roughly equally spaced arranged side by side respectively, is disposed in nozzle plate 28 with the state mutually staggering.Injector spacing in present embodiment is about 140 μ m.Therefore, from the orthogonal direction of nozzle rows 22,360 nozzles 21 become the state of arranging with the injector spacing of about 70 μ m.
For shower nozzle 20, if the drive waveforms as the signal of telecommunication of sending from shower nozzle drive division is applied to actuator, cause the volume variation of the chamber of pressurization part 27, with the pumping action producing therefrom, the functional layer being filled in chamber is formed with ink pressurization, functional layer formation is sprayed from the nozzle 21 being communicated with chamber with drop with ink.
Ink reservoir
Next, with reference to Fig. 3 and Fig. 5, the ink reservoir of present embodiment is described.Fig. 5 (a) is the stereogram that represents print cartridge, and Fig. 5 (b) is the fragmentary cross sectional view that represents the internal structure of print cartridge.
Ink reservoir can be the large container of inner capacities as the ink tank 14 shown in Fig. 3, but can not say long-time in ink tank 14 memory function layer to form be suitable with ink.Think if stored for a long time, for example functional layer form with solvent in ink reduce and the 3 one-tenth analyze, or viscosity variation, thus cannot stably spray drop from the nozzle of shower nozzle 20 21.Therefore, form with ink as object to supply with newer functional layer according to actual use amount, for example, can adopt the print cartridge 140 as ink reservoir shown in Fig. 5.
As shown in Fig. 5 (a), print cartridge 140 has the functional layer of accommodating and forms with the box main body 141 of the box of ink and the cap 143 sealing with box main body 141.Be provided with ink flow export 142 in the bottom of box main body 141.Be provided with the connected entrance 144 of the internal communication of the box main body 141 airtight with partes tegmentalis 143 at cap 143.
As shown in Fig. 5 (b), in the inside of box main body 141, be accommodated with porous member 145, functional layer formation is absorbed by porous member 145 with ink, is filled in box main body 141.Porous member 145 can use such as polyurathamc etc.
In the blowoff 1 of present embodiment, become the formation that 1 shower nozzle 20 has been installed at head cartridge 10, but be not limited to this, can become corresponding function layer and form the formation that multiple shower nozzles 20 are installed at head cartridge 10 by the kind of ink.Therefore, ink tank 14 or print cartridge 140 also corresponding function layer form prepare by the kind of ink multiple.In addition, can form in the mode that the print cartridge 140 more small-sized than ink tank 14 is arranged on to head cartridge 10, shorten the length of pipe arrangement 13, mobile shower nozzle 20 and print cartridge 140 simultaneously.
The manufacture method of organic EL
Next, with reference to Fig. 6, the manufacture method of the organic EL to present embodiment describes.Fig. 6 (a)～(d) is the fragmentary cross sectional view that represents the manufacture method of organic EL.
The manufacture method of the organic EL of present embodiment has: next door forms operation (step S1), surface treatment procedure (step S2), functional layer forms operation (step S3) and opposite electrode forms (step S4).Functional layer forms the formation method that operation (step S3) represents the functional layer of present embodiment.
Form in operation in the next door of step S1, as shown in Fig. 6 (a), on the device substrate 101 that is formed with pixel electrode 102, with the thickness coating of 1 μ m～2 μ m for example contain to functional layer form with ink show liquid repellency anti-liquid material photoresist material and be dried and form photo-sensitive resin.As coating process, can enumerate transfer printing, slit rubbing method etc.As anti-liquid material, can enumerate fluorine compounds, siloxane-based compound.As photoresist material, can enumerate the multifunctional acrylic resin of minus.Use the exposure mask corresponding with the shape of sub-pixel 110 to carry out exposure imaging to the photo-sensitive resin of making, form the next door 104 that overlaps with the outer rim of pixel electrode 102 and form peristome 104a on pixel electrode 102.Then, enter step S2.
In the surface treatment procedure of step S2, the device substrate 101 that is formed with next door 104 is implemented to surface treatment.Surface treatment procedure carries out in order to remove the refuses such as the surperficial next door residue of pixel electrode 102, object is that form functional layer by ink-jet method (drop ejection method) in next operation time, the functional layer that contains functional layer formation material forms with ink and can soak equably and expand the peristome 104a being impaled by next door 104.As surface treatment method, implement in the present embodiment Excimer uv (ultraviolet ray) and process.Should illustrate, surface treatment is not limited to Excimer uv processing, as long as can purify the surface of pixel electrode 102, for example, can utilize the cleaning-drying operation of solvent.In addition, if the surface of pixel electrode 102 is clean state, also can not implement surface treatment procedure.Then, enter step S3.
Form in operation in the functional layer of step S3, first, as shown in Fig. 6 (b), the hole injection layer formation ink 50 as functional layer formation ink that contains hole-injecting material is coated on to peristome 104a.Hole injection layer formation is used above-mentioned blowoff 1 with the coating process of ink 50.Hole injection layer formation is sprayed with drop D by the nozzle 21 from shower nozzle 20 with ink 50.The spray volume of the drop D spraying from shower nozzle 20 is pl unit and controlled, and the drop D of the number that ormal weight is obtained divided by the spray volume of drop D is sprayed onto peristome 104a.The hole injection layer being ejected forms uses ink 50 because swelling at peristome 104a with the surface tension in next door 104, but can not overflow.In other words,, to become the mode of ormal weight of the degree that can not overflow from peristome 104a, adjust in advance hole injection layer and form the concentration with the hole-injecting material (the 3rd composition) in ink 50.Then, enter drying process.
In drying process, for example form with the device substrate 101 of ink 50 and under reduced pressure places being coated with hole injection layer, make solvent evaporate and be dried (drying under reduced pressure) from hole injection layer formation ink 50., by under atmospheric pressure implement heat treated solidify, form hole injection layer 131 thereafter.For hole injection layer 131, in view of the selection of hole-injecting material described later, be not necessarily defined in this with the relation of other layer in functional layer 136, form with the thickness of about 20nm～40nm.
Next, use the hole transporting layer formation ink 60 as functional layer formation ink that contains hole transporting material to form hole transporting layer 132.The formation method of hole transporting layer 132 and hole injection layer 131 similarly use above-mentioned blowoff 1 to carry out., the hole transporting layer formation of ormal weight is sprayed onto to peristome 104a with drop D from the nozzle 21 of shower nozzle 20 with ink 60.Then, the hole transporting layer that is coated on peristome 104a is formed with ink 60 drying under reduced pressure.,, under the non-active gas atmosphere such as nitrogen, implement heat treated and form thus hole transporting layer 132 thereafter.For hole transporting layer 132, in view of the selection of hole transporting material described later, be not necessarily defined in this with the relation of other layer in functional layer 136, form with the thickness of about 20nm.
Next, use the luminescent layer formation ink 70 as functional layer formation ink that contains luminescent layer formation material to form luminescent layer 133.The formation method of luminescent layer 133 is also similarly used above-mentioned blowoff 1 to carry out with hole injection layer 131., the luminescent layer formation of ormal weight is sprayed to peristome 104a with drop D from the nozzle 21 of shower nozzle 20 with ink 70.Then, the luminescent layer that is coated on peristome 104a is formed with ink 70 drying under reduced pressure.,, under the non-active gas atmosphere such as nitrogen, implement heat treated and form thus luminescent layer 133 thereafter.For luminescent layer 133, in view of luminescent layer described later forms the selection of material, is not necessarily defined in this with the relation of other layer in functional layer 136, form with the thickness of about 30nm～80nm.
Next, cover luminescent layer 133 ground and form electron supplying layer 134.As the electron transport materials that forms electron supplying layer 134, be not particularly limited, in order to use the gas phase process such as vacuum vapour deposition to form, for example, can enumerate two (2-methyl-oxine-N1, O8)-(1,1 '-xenyl-4-hydroxyl) aluminium (BALq), 1,3,5-tri-(5-(4-tert-butyl-phenyl)-1,3,4-
diazole) (OXD-1), 2,9-dimethyl-4,7-diphenyl-1,10-ferrosin (BCP), (2-(4-xenyl)-5-(4-tert-butyl-phenyl)-1,2,4-
diazole (PBD), 3-(4-xenyl)-5-(4-tert-butyl-phenyl)-1,2,4-triazole (TAZ), 4,4 '-bis-(1,1-pair-diphenylacetylene) biphenyl (DPVBi), 2, two (the 1-naphthyls)-1,3 of 5-, 4-
diazole (BND), 4,4 '-bis-(two (4-aminomethyl phenyl) vinyl of 1,1-) biphenyl (DTVBi), 2, two (the 4-xenyls)-1,3 of 5-, 4-
diazole (BBD) etc.
In addition, can enumerate three (oxine) aluminium (Alq3),
oxadiazole derivative,
zole derivatives, ferrosin derivative, anthraquinone bismethane derivative, quinone derivatives, naphthoquinone derivatives, anthraquinone derivative, four cyano anthraquinone bismethane derivative, fluorene derivative, diphenyl dicyano ethene derivatives, diphenoquinone, 8-hydroxyquinoline derivative etc.Can use a kind in these or combine two or more use.
For electron supplying layer 134, in view of the selection of above-mentioned electron transport materials, be not necessarily defined in this with the relation of other layer in functional layer 136, form with the thickness of about 20nm～40nm.Thus, can will suitably be transported to luminescent layer 133 from opposite electrode 103 injected electrons as negative electrode.
Next, overlay electronic transfer layer 134 ground form electron injecting layer 135.As the electron injection material that forms electron injecting layer 135, be not particularly limited, in order to use the gas phase process such as vacuum vapour deposition to form, for example, can enumerate alkali metal compound, alkali earth metallic compound.
As alkali metal compound, for example, can enumerate LiF, Li
2cO
3, LiCl, NaF, Na
2cO
3, NaCl, CsF, Cs
2cO
3, the alkali metal salt such as CsCl.In addition, as alkali earth metallic compound, for example, can enumerate CaF
2, CaCO
3, SrF
2, SrCO
3, BaF
2, BaCO
3deng alkali earth metal salt.Can use a kind in these alkali metal compounds, alkali earth metallic compound or combine two or more use.
The thickness of electron injecting layer 135, is not particularly limited, and is preferably 0.01nm～10nm left and right, more preferably 0.1nm～5nm left and right.Thus, electronics can be injected into electron supplying layer 134 efficiently from the opposite electrode 103 as negative electrode.
Next, overlay electronic implanted layer 135 ground form the opposite electrode 103 as negative electrode.As the constituent material of opposite electrode 103, preferably use the little material of work function, and in order to use the gas phase process such as vacuum vapour deposition to form, for example, the alloy that can use Li, Mg, Ca, Sr, La, Ce, Er, Eu, Sc, Y, Yb, Ag, Cu, Al, Cs, Rb, Au or contain them etc., can use a kind in them or combine two or more (for example, multi-layer laminate etc.) and use.
Particularly, as present embodiment, when light-emitting device 100 is bottom emission mode, do not require that opposite electrode 103 has light transmission.Therefore, for example, preferably use the metal or alloy such as Al, Ag, AlAg, AlNd.By using the constituent material of such metal or alloy as opposite electrode 103, thereby can realize the electron injection efficiency of opposite electrode 103 and the raising of stability.
The thickness of opposite electrode 103 is not particularly limited, and is preferably 50nm～1000nm left and right, more preferably 100nm～500nm left and right.
When light-emitting device 100 is top emission design, as the constituent material of opposite electrode 103, preferably use the metal or alloy such as MgAg, MgAl, MgAu, AlAg.By using such metal or alloy, thereby the light transmission of opposite electrode 103 be can maintain, and the electron injection efficiency of opposite electrode 103 and the raising of stability realized.
The thickness of the opposite electrode 103 in top emission design is not particularly limited, and is preferably 1nm～50nm left and right, more preferably 5nm～20nm.
For the organic EL 130 of such formation, for example, if moisture, oxygen etc. immerse from outside, the lighting function of functional layer 136 is obstructed, and produces luminosity part and reduces or the not luminous dim spot forming (blackening).In addition, luminescent lifetime may shorten.Therefore,, in order to protect organic EL 130 to avoid the immersion of moisture, oxygen etc., preferably use sealant (omitting diagram) to cover.As sealant, for example, can use the inorganic insulating materials such as the silicon oxynitride (SiON) that the permeability of moisture, oxygen etc. is low.In addition, also the transparent hermetic sealing substrate such as glass, opaque pottery can be situated between and be fitted on the device substrate 101 that has formed organic EL 130 by bonding agent, sealing organic el element 130 thus.
In the manufacture method of above-mentioned organic EL 130, with hole injection layer 131, hole transporting layer 132 and luminescent layer 133 in liquid phase process (ink-jet method) formation functional layer 136, but as long as form 1 in these layers with liquid phase process (ink-jet method), other layer can use the gas phase process formation such as vacuum evaporation.
About hole injection layer 131, hole transporting layer 132, luminescent layer 133, the constituent material that can use in liquid phase process or gas phase process (the 3rd composition) is described.
Hole-injecting material
As the hole-injecting material that is suitable for forming above-mentioned hole injection layer 131, for example, can enumerate CuPc (CuPc), two ［ 4-(di-p-tolyl) aminophenyl ］ cyclohexanes (TAPC) of 1,1-, N, N '-diphenyl-N, N '-bis--(3-aminomethyl phenyl)-1,1 '-xenyl-4,4 '-diamines (TPD), N, N '-diphenyl-N, N '-bis--(1-naphthyl)-1,1 '-xenyl-4,4 '-diamines (α-NPD), 4,4 ', 4 "-tri-(N-3-aminomethyl phenyl amino) triphenylamine (m-MTDATA), 4,4 ', 4 "-tri-(N, N-(2-naphthyl) phenyl amino) triphenylamine (2-TNATA), 4,4 ', 4 "-tri-(N-carbazyl) triphenylamines (TCTA), 1,3,5-tri--(N, N-pair-(4-methoxyphenyl) aminophenyl) benzene (TDAPB), three (4-carbazole-9-base-phenyl) amine (spiro-TAD), DPPD (DTP), three para-totuidine (HTM1), two ［ (two-4-tolyl amino) phenyl ］ cyclohexanes (HTM2) of 1,1-, 1,3,5-tri-(4-pyridine radicals)-2,4,6-triazine (TPT1), triphenylamine tetramer (TPTE) etc.
Hole transporting material
As the hole transporting material that is suitable for forming above-mentioned hole transporting layer 132, for example, can use above-mentioned hole-injecting material.In addition, except above-mentioned hole-injecting material, for example, can enumerate TFB; The amine compounds such as the triphenylamine based polymer that (9,9-dioctyl-fluorenes-altogether-N-(4-butyl phenyl)-diphenylamines) is representative gathering, poly-fluorene derivative (PF), poly (phenylenevinylene) derivative (PPV), poly radical derivative (PPP), Polyvinyl carbazole (PVK), polythiofuran derivative, containing macromolecule organic materials such as the polysilane systems of Polymethylphenylsilane (PMPS).
Material of main part
As obtaining redness, green, shared material of main part in blue various luminous luminescent layers 133, can enumerate CBP (4, 4 '-bis-(9-bis-carbazyls)-2, 2 '-biphenyl), BAlq (two-(2-methyl-oxine)-4-(phenylphenol) aluminium), mCP (N, N-bis-carbazyl-3, 5-benzene: CBP derivative), CDBP (4, 4 '-bis-(9-carbazyls)-2, 2 '-dimethyl-biphenyl), DCB (N, N '-bis-carbazyl-1, 4-dimethylene-benzene), P06 (2, two (diphenyl phosphine oxide)-9 of 7-, 9-dimethyl fluorene), SimCP (3, two (9-carbazyl) tetraphenyl silane of 5-), UGH3 (two (triphenyl silicyl) benzene of W-), TDAPB (1, 3, 5-tri-［ 4-(diphenyl amino) phenyl ］ benzene etc.
Red illuminating material (dopant)
As the dopant (guest materials) that obtains emitting red light, can enumerate Bt2Ir (acac) (two (2-phenyl benzothiazole-N, C2 ') (acetylacetone,2,4-pentanedione) close iridium (III), Btp2Ir (acac) (two (2-2 '-benzothiophene)-pyridine-N, C3) (acetylacetone,2,4-pentanedione) closes the iridium complex compounds such as iridium, PtOEP (2,3,7,8,12,13,17,18-octaethyl-21H, the iridium-platinum complexes such as 23H-porphyrin platinum (II), thus can obtain red phosphorescence by adding in aforementioned body material.
As the high molecular red illuminating material (dopant) using in liquid phase process, can enumerate the fluorene derivatives such as chemical formula (1), (2).
Green luminescent material (dopant)
As the dopant (guest materials) that obtains green emitting, can enumerate Ir (ppy)
3(face formula-tri-(2-phenylpyridine) iridium), Ppy2Ir (acac) (two (2-phenyl-pyridine-N, C2) (acetylacetone,2,4-pentanedione) closes the iridium complex compounds such as iridium, thereby can obtain green phosphorescence by adding in aforementioned body material.
As the high molecular green luminescent material (dopant) using in liquid phase process, can enumerate the phenylene vinylidene derivatives such as chemical formula (3), (4).
Blue emitting material (dopant)
As the dopant (guest materials) that obtains blue-light-emitting, can enumerate FIrpic (two (4,6 difluorophenyls-pyridine-N, C.2.)-pyridine formyl closes iridium), ((1-phenyl-3-tolimidazole quinoline-2-pitches base-C to iridium-tri-to Ir (pmb) 3, C (2) '), FIrN4 (two (4,6-difluorophenyl pyridine) (5-(pyridine-2-yl)-tetrazolium closes iridium (III)), Firtaz (two (4,6-difluorophenyl pyridine) (5-(pyridine-2-yl)-1,2,4-triazole is closed iridium (III)) etc. iridium complex compound.Thereby add in aforementioned body material and can obtain blue phosphorescence by the dopant using these as guest materials.
In addition, guest materials when particularly conduct forms blue luminescent layer 133 with gas phase process such as vacuum evaporations, preferably uses the styryl derivatives such as chemical formula (5), (6), (7), (8).As material of main part, preferably use the anthracene derivants such as chemical formula (9), (10), (11).
In addition, as the luminescent material (dopant) that obtains fluorescence, can enumerate Alq
3(oxine) aluminium, rubrene, perylene, 9,10-diphenylanthrancene, tetraphenylbutadiene, Nile red, coumarin 6, quinacridone.
In addition, as the luminescent material (dopant) that can obtain blue fluorescence, can enumerate 1, two (2-methyl styrene base) benzene, 1 of 4-, 4-(3-methyl styrene base) benzene, 1,4-pair-(2-methyl styrene base) benzene, 1,4-(3-methyl styrene base) benzene, 1, two (the 4-methyl styrene base) benzene of 4-, diphenylethyllene benzene, 1, two (the 2-ethyl styrene base) benzene, 1 of 4-, two (the 3-ethyl styrene base) benzene of 4-, Isosorbide-5-Nitrae-bis-(2-methyl styrene base)-styryl benzene derivatives such as 2-methylbenzene.
Functional layer formation ink
Next, the functional layer formation of present embodiment is described by the formation of ink.Form respectively hole injection layer 131 in the functional layer 136 of organic EL 130 of present embodiment, hole transporting layer 132, luminescent layer 133 during with liquid phase process (ink-jet method), preferred functional layer forms with the basic comprising of ink as follows.
Functional layer forms the 1st composition that forms with ink at least a kind of aromatic solvent that to contain by boiling point be 250 ℃～350 ℃, is the 3rd composition that the 2nd composition that forms of 200 ℃ of at least a kind of above aliphatic solvents and functional layer form use by boiling point.Preferably the dissolubility of the 3rd composition is that the 1st composition is higher than the 2nd composition, and the mixing ratio of the 2nd composition is 30vol%～70vol%, and the boiling point of the 1st composition is higher than the boiling point of the 2nd composition, and the difference of the boiling point of the boiling point of the 1st composition and the 2nd composition is more than 30 ℃.
It is the aromatic solvent of 250 ℃～350 ℃ as the boiling point that can be used as the 1st composition, can enumerate 1,3-dipropoxy benzene (251 ℃ of boiling points), 4-methoxybenzaldehyde-dimethyl-acetal (253 ℃ of boiling points), 4,4 '-difluoro-diphenylmethane (258 ℃ of boiling points), diphenyl ether (259 ℃ of boiling points), 1,2-dimethoxy-4 '-(1-acrylic) benzene (264 ℃ of boiling points), MDPE (2-phenoxytoluene; 265 ℃ of boiling points), diphenyl-methane (265 ℃ of boiling points), 2-phenylpyridine (268 ℃ of boiling points), DMDPE (dimethyl phenylate; 270 ℃ of boiling points), 3-phenoxytoluene (272 ℃ of boiling points), 3-phenylpyridine (272 ℃ of boiling points), 2-phenyl methyl phenyl ethers anisole (274 ℃ of boiling points), 2-phenoxy group oxolane (275 ℃ of boiling points), NPBP (1-propyl group-4-phenyl benzene; 280 ℃ of boiling points), 25DMDPE (2-phenoxy group-Isosorbide-5-Nitrae-dimethylbenzene; 280 ℃ of boiling points), ethyl-2-naphthyl-ether (282 ℃ of boiling points), 225TMDPE (2,2,5-trimethyl diphenyl ether; 290 ℃ of boiling points), diphenyl ether (295 ℃ of boiling points), 235TMDPE (2,3,5-trimethyl diphenyl ether; 295 ℃ of boiling points), N-methyldiphenylamine (297 ℃ of boiling points), 4-isopropyl biphenyl (298 ℃ of boiling points), α, α-dichloro diphenyl methane (305 ℃ of boiling points), 4-(3-phenyl propyl) pyridine (322 ℃ of boiling points), Ergol (324 ℃ of boiling points), 1, two (3, the 4-3,5-dimethylphenyl) ethane (333 ℃ of boiling points) of 1-.
If considered as material of main part, the good dissolubility of dopant (guest materials) and the change of boiling point the 3rd composition, in hole-injecting material, hole transporting material, luminescent layer 133, be particularly preferably more than 270 ℃ 3-phenoxytoluene (272 ℃ of boiling points), diphenyl ether (295 ℃ of boiling points), 1 from boiling point, in two (3, the 4-3,5-dimethylphenyl) ethane (333 ℃ of boiling points) of 1-, select.
Be 200 ℃ of above aliphatic solvents as the boiling point that can be used as the 2nd composition, can enumerate the fatty ethers such as diethylene glycol butyl methyl ether (212 ℃ of boiling points), tripropylene glycol dimethyl ether (215 ℃ of boiling points), TRIGLYME (216 ℃ of boiling points), diethylene glycol monobutyl ether (230 ℃ of boiling points), dibutyl ethylene glycol ether (256 ℃ of boiling points), diethylene glycol butyl methyl ether (261 ℃ of boiling points), tetraethyleneglycol dimethyl ether (275 ℃ of boiling points).
In order to realize less than above-mentioned the 1st component list surface tension and to be the surface tension below 32mN/m, particularly preferably from diethylene glycol butyl methyl ether (212 ℃ of boiling points), dibutyl ethylene glycol ether (256 ℃ of boiling points), select.
If use the mixed solvent of the 1st composition of such aromatic solvent and the 2nd composition of aliphatic solvent, the boiling point of mixed solvent is more than 200 ℃, therefore after being filled into shower nozzle 20, under common operating environment, can occur hardly to make the 3 one-tenth obstructions that analyze the nozzle 21 causing because of functional layer formation ink setting in nozzle 21.In other words, can guarantee the ejection characteristic that shower nozzle 20 is stable., can realize the functional layer formation ink that is suitable for ink-jet method (drop ejection method).
In addition, in order to realize the desirable characteristics of luminescence in organic EL 130, need to be without the defect in film forming (there is no film forming in necessary region), with respect to target film thickness inequality or the few functional layer of deviation.Use as mentioned above the methods such as drying under reduced pressure to form with removing solvent composition ink from the functional layer that is ejected into the ormal weight of the peristome 104a in next door 104 from the nozzle 21 of shower nozzle 20 with drop D, form the functional layer being formed by the 3rd composition.Therefore the functional layer, being ejected forms and soaks expansion with ink equably at peristome 104a is important.The functional layer of present embodiment form with ink due to contain dissolubility excellence to the 3rd composition as the 1st composition of aromatic solvent and than the 1st component list surface tension little the 2nd composition as aliphatic solvent, so easily soak and expand in peristome 104a.
In addition, if before arriving the force drying operations such as drying under reduced pressure, heat drying, with being dried of natural drying promotion solvent composition, easily between the middle body on substrate W and outer peripheral portion, there is the uneven drying of solvent composition.So, the multiple peristome 104a on substrate W, the functional layer forming via force drying operation may produce thickness inequality, or thickness deviation becomes large.Form with for ink for the functional layer of present embodiment, because the boiling point of the mixed solvent that contains the 1st composition and the 2nd composition is more than 200 ℃, so be difficult to carry out natural drying, can reduce thickness inequality, the thickness deviation of the functional layer after force drying.
Below, enumerate concrete functional layer and form comparative example and the embodiment with ink, its evaluation result is described.
Should illustrate, it is to use the evaluation substrate that is formed with the next door 104 that forms 60000 peristome 104a that functional layer forms with the evaluation of ink, form and form 60000 organic ELs 130 with ink to this peristome 104a ejection functional layer, luminous bad these 3 the evaluation characteristics such as inequality, dim spot (blackening) or bright spot of the thickness by wetting extended defect, functional layer are evaluated.
Wetting extended defect is except comprising that the functional layer when being ejected into this peristome 104a forms the defect of the caused crawling of wetting expansion of use ink, also comprises by functional layer and forms with the cohesion of caused the 3rd composition of uneven drying of the solvent composition in the dry run of ink, the defect such as separates out.
Evaluate in characteristic for above-mentioned 3, wetting extended defect and luminous bad be that incidence is separately less than to 1% average evaluation is " ◎ ", be more than 1% and to be less than 5% average evaluation be "○", being more than 5% and being less than 10% average evaluation for " △ ", is that more than 10% average evaluation is "×".
The inequality of the thickness of functional layer is to be that average film thickness ± 1% is take inner evaluation as " ◎ " by the thickness of the central portion of this peristome 104a, for average film thickness ± 2.5% is take inner evaluation as "○", for average film thickness ± 5% is take inner evaluation as " △ ", the average evaluation that is greater than average film thickness ± 5% is "×".
< hole injection layer forms uses ink >
Fig. 7 represents that hole injection layer forms the formation of the comparative example 1-1～comparative example 1-25 that uses ink and the table of evaluation result.Fig. 8 represents that hole injection layer forms the formation of the comparative example 1-26～comparative example 1-50 that uses ink and the table of evaluation result.Fig. 9 represents that hole injection layer forms the formation of the comparative example 1-51～comparative example 1-75 that uses ink and the table of evaluation result.Figure 10 represents that hole injection layer forms the formation of the comparative example 1-76～comparative example 1-100 that uses ink and the table of evaluation result.Figure 11 represents that hole injection layer forms the formation of the embodiment 1-1～embodiment 1-25 that uses ink and the table of evaluation result.Figure 12 represents that hole injection layer forms comparative example 1-101～comparative example 1-116 and the formation of embodiment 1-26～embodiment 1-34 and the table of evaluation result with ink.Figure 13 represents that hole injection layer forms comparative example 1-117～comparative example 1-137 and the formation of embodiment 1-35～embodiment 1-38 and the table of evaluation result with ink.Figure 14 represents that hole injection layer forms the formation of the embodiment 1-39～embodiment 1-63 that uses ink and the table of evaluation result.Figure 15 represents that hole injection layer forms comparative example 1-138～comparative example 1-153 and the formation of embodiment 1-64～embodiment 1-72 and the table of evaluation result with ink.Figure 16 represents that hole injection layer forms comparative example 1-154～comparative example 1-174 and the formation of embodiment 1-73～embodiment 1-76 and the table of evaluation result with ink.Figure 17 represents that hole injection layer forms the formation of the embodiment 1-77～embodiment 1-101 that uses ink and the table of evaluation result.Figure 18 represents that hole injection layer forms comparative example 1-175～comparative example 1-190 and the formation of embodiment 1-102～embodiment 1-110 and the table of evaluation result with ink.Figure 19 represents that hole injection layer forms comparative example 1-191～comparative example 1-211 and the formation of embodiment 1-111～embodiment 1-114 and the table of evaluation result with ink.Figure 20 represents that hole injection layer forms the formation of the comparative example 1-212～comparative example 1-236 that uses ink and the table of evaluation result.Figure 21 represents that hole injection layer forms the formation of the comparative example 1-237～comparative example 1-261 that uses ink and the table of evaluation result.Figure 22 represents that hole injection layer forms the formation of the comparative example 1-262～comparative example 1-286 that uses ink and the table of evaluation result.Should illustrate, in the table of Fig. 7～Figure 22, the mode uprising gradually downwards from the top of table with boiling point as 25 kinds of aromatic solvents of illustrative the 1st composition is recorded.
Use each hole injection layer of comparative example 1-1～comparative example 1-286, embodiment 1-1～embodiment 1-114 to form with ink formation hole injection layer 131., utilize vapour deposition method, form hole transporting layer 132, luminescent layer 133, electron supplying layer 134, electron injecting layer 135 thereafter.The material of each layer is constructed as follows.Hole transporting layer 132 is α-NPD, and the material of main part of luminescent layer 133 is that CBP, dopant are Ir (ppy)
3, electron supplying layer 134 is BAlq, electron injecting layer 135 is LiF.
Comparative example 1-1～comparative example 1-25
As shown in Figure 7, the hole injection layer of comparative example 1-1～comparative example 1-25 form with ink be in each the 1st composition making as above-mentioned 25 kinds of aromatic solvents, contain 0.3wt% as 4 of hole-injecting material (the 3rd composition), 4 ', 4 "-tri-(N-3-aminomethyl phenyl-N-phenyl amino)-triphenylamine ［ m-MTDATA ］ forms.M-MTDATA is containing pi-conjugated low-molecular-weight organic compound.Do not contain the aliphatic solvent as the 2nd composition.In other words, each composition shared volume ratio in the mixed solvent of the 1st composition and the 2nd composition is that the 1st composition is 100vol%, and the 2nd composition is 0vol%.The 1st composition is the good solvent of the above-mentioned hole-injecting material of conduct the 3rd composition more than solubilized 0.1wt%.
It is poor that the hole injection layer of comparative example 1-1～comparative example 1-25 forms the wetting autgmentability of the pixel electrode being formed by ITO 102 to peristome 104a with ink, observes in the dry run of the 1st composition the state that pixel electrode 102 parts is exposed as the hole-injecting material cohesion of the 3rd composition.Wetting extended defect is "×".In addition, the degree of the thickness inequality of hole injection layer 131 is also bad, is " △ ", so because luminous bad this evaluation that takes place frequently is also "×".
(comparative example 1-26)～(comparative example 1-50)
As shown in Figure 8, the formation of the hole injection layer of comparative example 1-26～comparative example 1-50 is to coordinate to be the diethylene glycol butyl methyl ether of 212 ℃ and its m-MTDATA as hole-injecting material (the 3rd composition) that contains 0.3wt% is formed as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition with ink.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 80vol%, and the volume ratio of the 2nd composition is 20vol%.The boiling point of the 1st composition is higher than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is minimum 39 ℃～maximum 121 ℃.The dissolubility that the 2nd composition and the 1st composition compare the 3rd composition is low.In addition, the 2nd composition is less than the 1st component list surface tension.
The boiling point that contains 20vol% is under the diethylene glycol butyl methyl ether of the 212 ℃ state as the 2nd composition, with comparative example 1-1～comparative example 1-25 similarly, observe the state that pixel electrode 102 parts is exposed as the hole-injecting material cohesion of the 3rd composition.Wetting extended defect is "×".In addition, the degree of the thickness inequality of hole injection layer 131 is also " △ ", and luminous bad evaluation is also "×".
(comparative example 1-51)～(comparative example 1-75)
As shown in Figure 9, the formation of the hole injection layer of comparative example 1-51～comparative example 1-75 is to coordinate to be the dibutyl ethylene glycol ether of 256 ℃ and its m-MTDATA as hole-injecting material (the 3rd composition) that contains 0.3wt% is formed as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition with ink.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 80vol%, and the volume ratio of the 2nd composition is 20vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-5 ℃～77 ℃.The dissolubility that the 2nd composition and the 1st composition compare the 3rd composition is low.In addition, the 2nd composition is less than the 1st component list surface tension.
The boiling point that contains 20vol% is under the dibutyl ethylene glycol ether of the 256 ℃ state as the 2nd composition, with comparative example 1-1～comparative example 1-25 similarly, observe the state that pixel electrode 102 parts is exposed as the hole-injecting material cohesion of the 3rd composition.Wetting extended defect is "×".In addition, the degree of the thickness inequality of hole injection layer 131 is also " △ ", and luminous bad evaluation is also "×".
(comparative example 1-76)～(comparative example 1-100)
As shown in figure 10, to form with ink be that cooperation is the tetraethyleneglycol dimethyl ether of 275 ℃ and makes it contain 0.3wt% to form as the m-MTDATA of hole-injecting material (the 3rd composition) as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole injection layer of comparative example 1-76～comparative example 1-100.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 80vol%, and the volume ratio of the 2nd composition is 20vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-24 ℃～58 ℃.The dissolubility that the 2nd composition and the 1st composition compare the 3rd composition is low.In addition, the 2nd composition is less than the 1st component list surface tension.
The boiling point that contains 20vol% is under the tetraethyleneglycol dimethyl ether of the 275 ℃ state as the 2nd composition, with comparative example 1-1～comparative example 1-25 similarly, observe the state that pixel electrode 102 parts is exposed as the hole-injecting material cohesion of the 3rd composition.Wetting extended defect is "×".In addition, the degree of the thickness inequality of hole injection layer 131 is also " △ ", and luminous bad evaluation is also "×".
(embodiment 1-1)～(embodiment 1-25)
As shown in figure 11, to form with ink be that cooperation is the diethylene glycol butyl methyl ether of 212 ℃ and makes it contain 0.3wt% to form as the hole-injecting material m-MTDATA of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole injection layer of embodiment 1-1～embodiment 1-25.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 70vol%, and the volume ratio of the 2nd composition is 30vol%.In other words, embodiment 1-1～embodiment 1-25 has increased 10vol% by the volume ratio of the 2nd composition for comparative example 1-26～comparative example 1-50.
The hole injection layer of embodiment 1-1～embodiment 1-25 forms with ink by surface tension 2nd composition less than the 1st composition that contains 30vol%, thereby improves with the wetting autgmentability that comparative example 1-26～comparative example 1-50 compares peristome 104a.In addition, by boiling point 2nd composition lower than the 1st composition that contains 30vol%, thereby compared with comparative example 1-26～comparative example 1-50, in the drying under reduced pressure of solvent, maintain hole injection layer formation ink and be dried at the state of the wetting expansion of peristome 104a simultaneously, the thickness inequality of hole injection layer 131 also diminishes.Therefore the luminous bad generation such as dim spot, bright spot that, inhibition is caused by wetting extended defect, thickness inequality.In the poor Δ bp of the boiling point of the 1st composition and the boiling point of the 2nd composition is embodiment 1-1～embodiment 1-21 of 39 ℃～86 ℃, 3 assessment items are "○".In the poor Δ bp of boiling point is embodiment 1-22～embodiment 1-25 of 98 ℃～121 ℃, uneven and luminous bad being evaluated as " △ " of thickness.Think that this is because because the boiling point of the 1st composition is greater than 300 ℃, thus be difficult to make the aromatic solvent of the 1st composition to evaporate equably, but think and for example, can improve by revising drying condition (, the decompression degree in drying under reduced pressure etc.).
(comparative example 1-101)～(comparative example 1-116)
As shown in figure 12, the hole injection layer of comparative example 1-101～comparative example 1-116 forms and is lower each the 1st composition of 16 kinds of the above-mentioned 25 kinds of aromatic solvent mid-boiling points of cooperation and is the dibutyl ethylene glycol ether of 256 ℃ and makes it contain 0.3wt% to form as the m-MTDATA of hole-injecting material (the 3rd composition) as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition with ink.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 70vol%, and the volume ratio of the 2nd composition is 30vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-5 ℃～26 ℃.The dissolubility that the 2nd composition and the 1st composition compare the 3rd composition is low.In addition, the 2nd composition is less than the 1st component list surface tension.
Even if the hole injection layer that the 1st composition and the poor Δ bp of the boiling point of the 2nd composition are comparative example 1-101～comparative example 1-116 of-5 ℃～26 ℃ forms surface tension 2nd composition less than the 1st composition that contains 30vol% with ink, also can observe wetting extended defect.Wetting extended defect, thickness inequality and luminous bad degree are along with the poor Δ bp of boiling point becomes large and improves, but it is evaluated as "×"～" △ ".
(embodiment 1-26)～(embodiment 1-34)
As shown in figure 12, the formation of the hole injection layer of embodiment 1-26～embodiment 1-34 is coordinate each the 1st composition of 9 kinds that 25 kinds of above-mentioned aromatic solvent mid-boiling points are higher and be the dibutyl ethylene glycol ether of 256 ℃ and its m-MTDATA as hole-injecting material (the 3rd composition) that contains 0.3wt% is formed as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition with ink.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 70vol%, and the volume ratio of the 2nd composition is 30vol%.In other words, embodiment 1-26～embodiment 1-34 has increased 10vol% by the volume ratio of the 2nd composition for comparative example 1-67～comparative example 1-75.
The 1st composition and the poor Δ bp of the boiling point of the 2nd composition are that the hole injection layer of embodiment 1-26～embodiment 1-34 of 34 ℃～77 ℃ forms with ink by surface tension 2nd composition less than the 1st composition that contains 30vol%, thereby make to compare and improve with comparative example 1-101～comparative example 1-116 with comparative example 1-67～comparative example 1-75 in the wetting autgmentability of peristome 104a.The evaluation of wetting extended defect is "○".The evaluation of thickness inequality is embodiment 1-26～embodiment 1-29 is " ◎ ", and embodiment 1-30 is "○", and it is just still " △ " that the boiling point of the 1st composition is greater than embodiment 1-31～embodiment 1-34 of 300 ℃.Luminous bad evaluation is that embodiment 1-26～embodiment 1-30 is "○", and it is just still " △ " that the boiling point of the 1st composition is greater than embodiment 1-31～embodiment 1-34 of 300 ℃.Thickness inequality and luminous bad being evaluated as " △ " can improve by changing drying under reduced pressure condition as mentioned above.
(comparative example 1-117)～(comparative example 1-137)
As shown in figure 13, the formation of the hole injection layer of comparative example 1-117～comparative example 1-137 is coordinate each the 1st composition of 21 kinds that above-mentioned 25 kinds of aromatic solvent mid-boiling points are lower and be the tetraethyleneglycol dimethyl ether of 275 ℃ and its m-MTDATA as hole-injecting material (the 3rd composition) that contains 0.3wt% is formed as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition with ink.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 70vol%, and the volume ratio of the 2nd composition is 30vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-24 ℃～23 ℃.The dissolubility that the 2nd composition and the 1st composition compare the 3rd composition is low.In addition, the 2nd composition is less than the 1st component list surface tension.
Even if the hole injection layer that the 1st composition and the poor Δ bp of the boiling point of the 2nd composition are comparative example 1-117～comparative example 1-137 of-24 ℃～23 ℃ forms surface tension 2nd composition less than the 1st composition that contains 30vol% with ink, also can observe wetting extended defect.Wetting extended defect, thickness inequality and luminous bad degree are along with the poor Δ bp of boiling point becomes large and improves, but it is evaluated as "×"～" △ ".
(embodiment 1-35)～(embodiment 1-38)
As shown in figure 13, the hole injection layer of embodiment 1-35～embodiment 1-38 forms and is higher each the 1st composition of 4 kinds of the above-mentioned 25 kinds of aromatic solvent mid-boiling points of cooperation and is the tetraethyleneglycol dimethyl ether of 275 ℃ and makes it contain 0.3wt% to form as the m-MTDATA of hole-injecting material (the 3rd composition) as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition with ink.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 70vol%, and the volume ratio of the 2nd composition is 30vol%.In other words, embodiment 1-35～embodiment 1-38 has increased 10vol% by the volume ratio of the 2nd composition for comparative example 1-97～comparative example 1-100.
The 1st composition and the poor Δ bp of the boiling point of the 2nd composition are that the hole injection layer of embodiment 1-35～embodiment 1-38 of 30 ℃～58 ℃ forms with ink by surface tension 2nd composition less than the 1st composition that contains 30vol%, thereby make to compare and improve with comparative example 1-117～comparative example 1-137 with comparative example 1-97～comparative example 1-100 in the wetting autgmentability of peristome 104a.The evaluation of wetting extended defect is "○".So because being greater than 300 ℃, the boiling point of the 1st composition is difficult to evenly carry out the dry of mixed solvent as mentioned above, thickness inequality and luminous bad being evaluated as " △ ", but can improve by revising drying under reduced pressure condition.
(embodiment 1-39)～(embodiment 1-63)
As shown in figure 14, the hole injection layer of embodiment 1-39～embodiment 1-63 form with ink be using as each the 1st composition of above-mentioned 25 kinds of aromatic solvents and as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition be the diethylene glycol butyl methyl ether of 212 ℃ using volume ratio respectively as 50vol% coordinates and its m-MTDATA as hole-injecting material as the 3rd composition that contains 0.3wt% is formed.In other words, for comparative example 1-26～comparative example 1-50, the volume ratio of the 2nd composition has been increased to 30vol%.In other words, compared with embodiment 1-1～embodiment 1-25, the volume ratio of the 2nd composition has been increased to 20vol%.
The hole injection layer formation of embodiment 1-39～embodiment 1-63, improves thereby make that peristome 104a is soaked to autgmentability by surface tension the 2nd composition less than the 1st composition that contains 50vol% with ink compared with comparative example 1-26～comparative example 1-50.In addition, by boiling point 2nd composition lower than the 1st composition that contains 50vol%, thereby compared with comparative example 1-26～comparative example 1-50, in drying under reduced pressure, maintain hole injection layer formation ink and be dried at the state of the wetting expansion of peristome 104a simultaneously, the thickness inequality of hole injection layer 131 also diminishes.In addition, compared with embodiment 1-22～embodiment 1-25, even if being greater than 300 ℃, the boiling point of the 1st composition is also difficult for producing thickness inequality.Therefore, suppressed the luminous bad generation such as dim spot, bright spot that caused by wetting extended defect, thickness inequality.So, evaluate characteristic for 3 and be "○".
(comparative example 1-138)～(comparative example 1-153)
As shown in figure 15, the hole injection layer of comparative example 1-138～comparative example 1-153 form with ink be using each the 1st composition of 16 kinds lower above-mentioned 25 kinds of aromatic solvent mid-boiling points and the dibutyl ethylene glycol ether that is 256 ℃ as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition coordinates and makes it contain 0.3wt% using each 50vol% and forms as the m-MTDATA as hole-injecting material of the 3rd composition.
Even if the 1st composition forms with the surface tension that contains 50vol% in ink 2nd composition less than the 1st composition with the hole injection layer that the poor Δ bp of the boiling point of the 2nd composition is comparative example 1-138～comparative example 1-153 of-5 ℃～26 ℃, also can observe wetting extended defect.Wetting extended defect, thickness inequality and luminous bad degree are along with the poor Δ bp of boiling point becomes large and improves, but it is evaluated as "×"～" △ ".
(embodiment 1-64)～(embodiment 1-72)
As shown in figure 15, the hole injection layer of embodiment 1-64～embodiment 1-72 form with ink be using each the 1st composition of 9 kinds higher above-mentioned 25 kinds of aromatic solvent mid-boiling points and the dibutyl ethylene glycol ether that is 256 ℃ as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition coordinates and its m-MTDATA as hole-injecting material as the 3rd composition that contains 0.3wt% is formed using each 50vol%.In other words, for comparative example 1-67～comparative example 1-75, the 2nd composition has been increased to 30vol% in volume ratio.
By being that the hole injection layer of embodiment 1-64～embodiment 1-72 of 34 ℃～77 ℃ forms with the surface tension that contains 50vol% in ink 2nd composition less than the 1st composition at the 1st composition and the poor Δ bp of the boiling point of the 2nd composition, thereby make to compare and improve with comparative example 1-138～comparative example 1-153 with comparative example 1-67～comparative example 1-75 in the wetting autgmentability of peristome 104a.The evaluation of wetting extended defect is "○".The evaluation of thickness inequality is that embodiment 1-64～embodiment 1-67 is " ◎ ", and embodiment 1-68 and embodiment 1-69 are "○", and embodiment 1-70～embodiment 1-72 is " △ ".Luminous bad evaluation is "○".
(comparative example 1-154)～(comparative example 1-174)
As shown in figure 16, the hole injection layer of comparative example 1-154～comparative example 1-174 form with ink be using each the 1st composition of 21 kinds lower above-mentioned 25 kinds of aromatic solvent mid-boiling points and the tetraethyleneglycol dimethyl ether that is 275 ℃ as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition coordinates and makes it contain 0.3wt% using each 50vol% and forms as the m-MTDATA as hole-injecting material of the 3rd composition.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-24 ℃～23 ℃.The dissolubility that the 2nd composition and the 1st composition compare the 3rd composition is low.In addition, the 2nd composition is compared with the 1st composition, and surface tension is little.
Even if the hole injection layer that is comparative example 1-154～comparative example 1-174 of-24 ℃～23 ℃ at the 1st composition and the poor Δ bp of the boiling point of the 2nd composition forms with the surface tension that contains 50vol% in ink 2nd composition less than the 1st composition, also can observe wetting extended defect.Wetting extended defect, thickness inequality and luminous bad degree are along with the poor Δ bp of boiling point becomes large and improves, but it is evaluated as "×"～" △ ".
(embodiment 1-73)～(embodiment 1-76)
As shown in figure 16, the hole injection layer of embodiment 1-73～embodiment 1-76 form with ink be using each the 1st composition of 4 kinds higher above-mentioned 25 kinds of aromatic solvent mid-boiling points and the tetraethyleneglycol dimethyl ether that is 275 ℃ as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition coordinates and its m-MTDATA as hole-injecting material as the 3rd composition that contains 0.3wt% is formed using each 50vol%.In other words, for comparative example 1-97～comparative example 1-100, the volume ratio of the 2nd composition has been increased to 30vol%.In other words, for embodiment 1-35～embodiment 1-38, the volume ratio of the 2nd composition has been increased to 20vol%.
By being that the hole injection layer of embodiment 1-73～embodiment 1-76 of 30 ℃～58 ℃ forms with the surface tension that contains 50vol% in ink 2nd composition less than the 1st composition at the 1st composition and the poor Δ bp of the boiling point of the 2nd composition, thereby make to compare and improve with comparative example 1-154～comparative example 1-174 with comparative example 1-97～comparative example 1-100 in the wetting autgmentability of peristome 104a.The evaluation of wetting extended defect is "○".So be difficult to carry out equably the dry of mixed solvent because the boiling point of the 1st composition is greater than 300 ℃ as mentioned above, so thickness is uneven and luminous bad being evaluated as " △ ".The evaluation of 3 assessment items is identical with embodiment 1-35～embodiment 1-38.
(embodiment 1-77)～(embodiment 1-101)
As shown in figure 17, the hole injection layer of embodiment 1-77～embodiment 1-101 form with ink be cooperation as each the 1st composition of above-mentioned 25 kinds of aromatic solvents and as above-mentioned the 2nd composition 7 kinds of aliphatic solvent mid-boiling points be the diethylene glycol butyl methyl ether of 212 ℃ and make it contain 0.3wt% to form as the m-MTDATA as hole-injecting material of the 3rd composition.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 30vol%, and the volume ratio of the 2nd composition is 70vol%.In other words, for embodiment 1-39～embodiment 1-63, the volume ratio of the 2nd composition has further been increased to 20vol%.
Even if the hole injection layer that the 1st composition and the poor Δ bp of the boiling point of the 2nd composition are embodiment 1-77～embodiment 1-101 of 39 ℃～121 ℃ forms surface tension 2nd composition less than the 1st composition that contains 70vol% with ink, wetting autgmentability at peristome 104a is also same with embodiment 1-39～embodiment 1-63, and the evaluation of wetting extended defect is "○".Thickness inequality and luminous bad evaluation are in embodiment 1-77～embodiment 1-97, to be "○".The boiling point of the 1st composition is greater than in the embodiment 1-98～embodiment 101 of 300 ℃, in drying under reduced pressure, be difficult to carry out equably being dried after the 2nd composition evaporation, so thickness is uneven and luminous bad being evaluated as " △ ", but can improve by revising drying under reduced pressure condition.
(comparative example 1-175)～(comparative example 1-190)
As shown in figure 18, the hole injection layer of comparative example 1-175～comparative example 1-190 forms and is lower each the 1st composition of 16 kinds of the above-mentioned 25 kinds of aromatic solvent mid-boiling points of cooperation and is the dibutyl ethylene glycol ether of 256 ℃ and makes it contain 0.3wt% to form as the m-MTDATA as hole-injecting material of the 3rd composition as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition with ink.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 30vol%, and the volume ratio of the 2nd composition is 70vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-5 ℃～26 ℃.The dissolubility that the 2nd composition and the 1st composition compare the 3rd composition is low.In addition, the 2nd composition is less than the 1st component list surface tension.
Even if the hole injection layer that is comparative example 1-175～comparative example 1-190 of-5 ℃～26 ℃ at the 1st composition and the poor Δ bp of the boiling point of the 2nd composition forms with the surface tension that contains 70vol% in ink 2nd composition less than the 1st composition, also can observe wetting extended defect.Wetting extended defect, thickness inequality and luminous bad degree are along with the poor Δ bp of boiling point becomes large and improves, but it is evaluated as "×"～" △ ".
(embodiment 1-102)～(embodiment 1-110)
As shown in figure 18, the hole injection layer of embodiment 1-102～embodiment 1-110 forms and is higher each the 1st composition of 9 kinds of the above-mentioned 25 kinds of aromatic solvent mid-boiling points of cooperation and is the dibutyl ethylene glycol ether of 256 ℃ and makes it contain 0.3wt% to form as the m-MTDATA as hole-injecting material of the 3rd composition as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition with ink.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 30vol%, and the volume ratio of the 2nd composition is 70vol%.In other words, compared with comparative example 1-67～comparative example 1-75, the volume ratio of the 2nd composition has been increased to 50vol%.Compared with embodiment 1-64～embodiment 1-72, the volume ratio of the 2nd composition is increased to 20vol%.
By being that the hole injection layer of embodiment 1-102～embodiment 1-110 of 34 ℃～77 ℃ forms with the surface tension that contains 70vol% in ink 2nd composition less than the 1st composition at the 1st composition and the poor Δ bp of the boiling point of the 2nd composition, thereby make to compare and improve with comparative example 1-175～comparative example 1-190 with comparative example 1-67～comparative example 1-75 in the wetting autgmentability of peristome 104a.The evaluation of wetting extended defect is "○".The evaluation of thickness inequality is embodiment 1-102～embodiment 1-105 is " ◎ ", and embodiment 1-106 is "○", and it is just still " △ " that the boiling point of the 1st composition is greater than embodiment 1-107～embodiment 1-110 of 300 ℃.Luminous bad evaluation is that embodiment 1-102～embodiment 1-106 is "○", and it is just still " △ " that the boiling point of the 1st composition is greater than embodiment 1-107～embodiment 1-110 of 300 ℃.Thickness inequality and the luminous bad evaluation for " △ " can improve by revising drying under reduced pressure condition as mentioned above.
(comparative example 1-191)～(comparative example 1-211)
As shown in figure 19, the hole injection layer of comparative example 1-191～comparative example 1-211 forms and is each the 1st composition of 21 kinds that the above-mentioned 25 kinds of aromatic solvent mid-boiling points of cooperation are lower and is the tetraethyleneglycol dimethyl ether of 275 ℃ and makes it contain 0.3wt% to form as the m-MTDATA of hole-injecting material (the 3rd composition) as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition with ink.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 30vol%, and the volume ratio of the 2nd composition is 70vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-24 ℃～23 ℃.The dissolubility that the 2nd composition and the 1st composition compare the 3rd composition is low.In addition, the 2nd composition is less than the 1st component list surface tension.
Even if the hole injection layer that is comparative example 1-191～comparative example 1-211 of-24 ℃～23 ℃ at the 1st composition and the poor Δ bp of the boiling point of the 2nd composition forms with the surface tension that contains 70vol% in ink 2nd composition less than the 1st composition, also can observe wetting extended defect.Wetting extended defect, thickness inequality and luminous bad degree are along with the poor Δ bp of boiling point becomes large and improves, but it is evaluated as "×"～" △ ".
(embodiment 1-111)～(embodiment 1-114)
As shown in figure 19, the hole injection layer of embodiment 1-111～embodiment 1-114 forms and is higher each the 1st composition of 4 kinds of the above-mentioned 25 kinds of aromatic solvent mid-boiling points of cooperation and is the tetraethyleneglycol dimethyl ether of 275 ℃ and makes it contain 0.3wt% to form as the m-MTDATA of hole-injecting material (the 3rd composition) as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition with ink.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 30vol%, and the volume ratio of the 2nd composition is 70vol%.In other words, for comparative example 1-97～comparative example 1-100, the volume ratio of the 2nd composition has been increased to 50vol%.In other words, compared with embodiment 1-73～embodiment 1-76, the volume ratio of the 2nd composition has been increased to 20vol%.
The 1st composition and the poor Δ bp of the boiling point of the 2nd composition are that the hole injection layer of embodiment 1-111～embodiment 1-114 of 30 ℃～58 ℃ forms with ink by surface tension 2nd composition less than the 1st composition that contains 70vol%, thereby make to improve compared with comparative example 1-191～comparative example 1-211 in the wetting autgmentability of peristome 104a.The evaluation and the identical "○" that is of embodiment 1-73～embodiment 1-76 of wetting extended defect.So because being greater than 300 ℃, the boiling point of the 1st composition is difficult to carry out equably the dry of mixed solvent, thickness inequality and luminous bad being evaluated as " △ ", but can improve by revising drying under reduced pressure condition.
(comparative example 1-212)～(comparative example 1-236)
As shown in figure 20, to form with ink be that cooperation is the diethylene glycol butyl methyl ether of 212 ℃ and makes it contain 0.3wt% to form as the m-MTDATA as hole-injecting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole injection layer of comparative example 1-212～comparative example 1-236.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 20vol%, and the volume ratio of the 2nd composition is 80vol%.The boiling point of the 1st composition is higher than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is 39 ℃～121 ℃.The dissolubility that the 2nd composition and the 1st composition compare the 3rd composition is low.In addition, the 2nd composition is less than the 1st component list surface tension.
By being that the hole injection layer of comparative example 1-212～comparative example 1-236 of 39 ℃～121 ℃ forms with the surface tension that contains 80vol% in ink 2nd composition less than the 1st composition at the 1st composition and the poor Δ bp of the boiling point of the 2nd composition, thereby soak the "○" that is evaluated as of extended defect.But 2nd composition lower than the 1st composition at drying under reduced pressure mid-boiling point first evaporates, the amount of the 1st remaining composition tails off compared with embodiment 1-77～embodiment 1-101, thus occur the 3rd composition cohesion, separate out and make thickness inequality.Therefore, the uneven and luminous bad "×" that is evaluated as of thickness.
(comparative example 1-237)～(comparative example 1-261)
As shown in figure 21, to form with ink be that cooperation is the dibutyl ethylene glycol ether of 256 ℃ and makes it contain 0.3wt% to form as the m-MTDATA of hole-injecting material (the 3rd composition) as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole injection layer of comparative example 1-237～comparative example 1-261.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 20vol%, and the volume ratio of the 2nd composition is 80vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-5 ℃～77 ℃.The dissolubility that the 2nd composition and the 1st composition compare the 3rd composition is low.In addition, the 2nd composition is less than the 1st component list surface tension.
Even if the hole injection layer that the 1st composition and the poor Δ bp of the boiling point of the 2nd composition are comparative example 1-237～comparative example 1-252 of-5 ℃～26 ℃ forms surface tension 2nd composition less than the 1st composition that contains 80vol% with ink, also can observe wetting extended defect, it is evaluated as along with the poor Δ bp of boiling point becomes large and improves, but is "×"～" △ ".The 1st composition and the poor Δ bp of the boiling point of the 2nd composition are that the hole injection layer of 34 ℃ of above comparative example 1-253～comparative example 1-261 forms with ink by surface tension 2nd composition less than the 1st composition that contains 80vol%, thereby be difficult to produce wetting extended defect, it is evaluated as "○".But, in comparative example 1-237～comparative example 1-261, in drying under reduced pressure, follow the amount of remaining the 1st composition after the 2nd composition evaporation to reduce and occur the 3rd composition cohesion, separate out the uneven and luminous bad "×" that is evaluated as of thickness.
(comparative example 1-262)～(comparative example 1-286)
As shown in figure 22, to form with ink be that cooperation is the tetraethyleneglycol dimethyl ether of 275 ℃ and makes it contain 0.3wt% to form as the m-MTDATA of hole-injecting material (the 3rd composition) as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole injection layer of comparative example 1-262～comparative example 1-286.The volume ratio of the 1st composition in the mixed solvent of the 1st composition and the 2nd composition is 20vol%, and the volume ratio of the 2nd composition is 80vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-24 ℃～58 ℃.The dissolubility that the 2nd composition and the 1st composition compare the 3rd composition is low.In addition, the 2nd composition is less than the 1st component list surface tension.
Even if the hole injection layer that the 1st composition and the poor Δ bp of the boiling point of the 2nd composition are comparative example 1-262～comparative example 1-282 of-24 ℃～23 ℃ forms surface tension 2nd composition less than the 1st composition that contains 80vol% with ink, also can observe wetting extended defect, it is evaluated as along with the poor Δ bp of boiling point becomes large and improves, but is "×"～" △ ".The 1st composition and the poor Δ bp of the boiling point of the 2nd composition are that the hole injection layer of 30 ℃ of above comparative example 1-283～comparative example 1-286 forms with ink by surface tension 2nd composition less than the 1st composition that contains 80vol%, thereby be difficult to produce wetting extended defect, it is evaluated as "○".But, in comparative example 1-262～comparative example 1-286, in drying under reduced pressure, occur along with the amount of remaining the 1st composition after the 2nd composition evaporation reduces the 3rd composition cohesion, separate out the uneven and luminous bad "×" that is evaluated as of thickness.
For the hole injection layer formation ink of above-mentioned comparative example and embodiment, evaluation result is summarized as to following content.
Because hole injection layer formation is coated on the pixel electrode 102 being formed by ITO in the peristome 104a in next door 104 with ink, so it is poor not contain as the wetting autgmentability of comparative example 1-1～comparative example 1-25 of the 2nd composition of aliphatic solvent, can not get the hole injection layer 131 of desirable thickness.In addition, in comparative example 1-26～comparative example 1-100 that the volume ratio of the 2nd composition is 20vol%, still just obtain the poor this same evaluation result of wetting autgmentability on pixel electrode 102.In addition, in the comparative example 1-212～comparative example 1-286 that is 80vol% at the volume ratio of the 2nd composition, the poor Δ bp of the boiling point of the 1st composition and the 2nd composition is wetting favorable expandability when more than 30 ℃, but the poor Δ bp of boiling point be less than 30 ℃ or the 2nd composition higher than the 1st composition boiling point, wetting autgmentability obviously declines.In comparative example 1-212～comparative example 1-286, all cannot form the hole injection layer 131 with target film thickness.
On the other hand, in embodiment 1-1～embodiment 1-114, from 25 kinds of aromatic solvents, select the 1st composition take the boiling point poor Δ bp higher than the boiling point of the 2nd composition and boiling point of the 1st composition as more than 30 ℃ modes, from 3 kinds of aliphatic solvents, select the 2nd composition.The volume ratio of the 2nd composition in the mixed solvent that in addition, contains the 1st composition and the 2nd composition is 30vol%～70vol%.Form the formation with the mixed solvent of ink by becoming such hole injection layer, even if thereby use low molecular hole-injecting material as the 3rd composition, also can guarantee the wetting autgmentability on pixel electrode 102, and in drying under reduced pressure, reduce as the cohesion of the m-MTDATA of the low molecular material of conduct of the 3rd composition, separate out and form the hole injection layer 131 that thickness is uneven few.
In embodiment 1-1～embodiment 1-114, from (2,2, the 5-trimethyl diphenyl ether of the 225TMDPE as aromatic solvent; 290 ℃ of boiling points), diphenyl ether (295 ℃ of boiling points), 235TMDPE (2,3,5-trimethyl diphenyl ether; 295 ℃ of boiling points), select the 1st composition in N-methyldiphenylamine (297 ℃ of boiling points), selecting boiling point is that the dibutyl ethylene glycol ether of 256 ℃ is as the 2nd composition, the volume ratio of the 2nd composition is that embodiment 1-26～embodiment 1-29, the embodiment 1-64～embodiment 1-67 of 30vol%～50vol% can form more uniform hole injection layer 131, so preferably.
Comparative example 1-101～comparative example 1-211 and embodiment 1-1～embodiment 1-114 similarly make the scope that the volume ratio of the 2nd composition in mixed solvent is 30vol%～70vol%, but when the 1st composition is less than 30 ℃ with the poor Δ bp of the boiling point of the 2nd composition or the 2nd composition than the 1st composition boiling point when high, wetting autgmentability obviously declines and produces thickness inequality compared with embodiment 1-1～embodiment 1-114.
Hole transporting layer formation ink
Figure 23 represents that hole transporting layer forms the formation of the comparative example 2-1～comparative example 2-25 that uses ink and the table of evaluation result.Figure 24 represents that hole transporting layer forms the formation of the comparative example 2-26～comparative example 2-50 that uses ink and the table of evaluation result.Figure 25 represents that hole transporting layer forms the formation of the comparative example 2-51～comparative example 2-75 that uses ink and the table of evaluation result.Figure 26 represents that hole transporting layer forms the formation of the comparative example 2-76～comparative example 2-100 that uses ink and the table of evaluation result.Figure 27 represents that hole transporting layer forms the formation of the embodiment 2-1～embodiment 2-25 that uses ink and the table of evaluation result.Figure 28 represents that hole transporting layer forms comparative example 2-101～comparative example 2-116 and the formation of embodiment 2-26～embodiment 2-34 and the table of evaluation result with ink.Figure 29 represents that hole transporting layer forms comparative example 2-117～comparative example 2-137 and the formation of embodiment 2-35～embodiment 2-38 and the table of evaluation result with ink.Figure 30 represents that hole transporting layer forms the formation of the embodiment 2-39～embodiment 2-63 that uses ink and the table of evaluation result.Figure 31 represents that hole transporting layer forms comparative example 2-138～comparative example 2-153 and the formation of embodiment 2-64～embodiment 2-72 and the table of evaluation result with ink.Figure 32 represents that hole transporting layer forms comparative example 2-154～comparative example 2-174 and the formation of embodiment 2-73～embodiment 2-76 and the table of evaluation result with ink.Figure 33 represents that hole transporting layer forms the formation of the embodiment 2-77～embodiment 2-101 that uses ink and the table of evaluation result.Figure 34 represents that hole transporting layer forms comparative example 2-175～comparative example 2-190 and the formation of embodiment 2-102～embodiment 2-110 and the table of evaluation result with ink.Figure 35 represents that hole transporting layer forms comparative example 2-191～comparative example 2-211 and the formation of embodiment 2-111～embodiment 2-114 and the table of evaluation result with ink.Figure 36 represents that hole transporting layer forms the formation of the comparative example 2-212～comparative example 2-236 that uses ink and the table of evaluation result.Figure 37 represents that hole transporting layer forms the formation of the comparative example 2-237～comparative example 2-261 that uses ink and the table of evaluation result.Figure 38 represents that hole transporting layer forms the formation of the comparative example 2-262～comparative example 2-286 that uses ink and the table of evaluation result.Should illustrate, in the table of Figure 23～Figure 37, as 25 kinds of aromatic solvents of the 1st composition to be recorded from the top mode that boiling point raises successively downwards of table.
The hole transporting layer of comparative example 2-1～comparative example 2-286, embodiment 2-1～embodiment 2-114 forms uses ink and above-mentioned hole injection layer formation ink similarly, from 25 kinds of aromatic solvents, select the 1st composition, from 3 kinds of aliphatic solvents, select the 2nd composition, the volume ratio that changes each composition utilizes ink-jet method to form hole transporting layer 132.Particularly, first, utilize liquid phase process (ink-jet method) to form hole injection layer 131.,, use each hole transporting layer of comparative example 2-1～comparative example 2-286, embodiment 2-1～embodiment 2-114 to form with ink formation hole transporting layer 132 thereafter.Then, utilize vapour deposition method, form luminescent layer 133, electron supplying layer 134, electron injecting layer 135.The material of each layer is constructed as follows.Hole injection layer 131 is PEDOT/PSS; Poly-(3,4-rthylene dioxythiophene)-poly-(styrene sulfonic acid), hole transporting layer 132 is TFB, and the material of main part of luminescent layer 133 is CBP, and dopant is Ir (ppy)
3, electron supplying layer 134 is BAlq, electron injecting layer 135 is LiF.
The hole transporting layer of comparative example 2-1～comparative example 2-286, embodiment 2-1～embodiment 2-114 form form by the situation of ink with the evaluation method of ink and above-mentioned hole injection layer identical, based on wetting expand owe to fall into, the inequality of thickness, luminous bad these 3 assessment items evaluate.Wherein, except evaluating forming the uneven caused defect of thickness with the hole injection layer 131 of ink by being coated with hole transporting layer.Luminous too bad.
(comparative example 2-1)～(comparative example 2-25)
As shown in figure 23, it is in each the 1st composition making as above-mentioned 25 kinds of aromatic solvents, to contain 0.5wt% to form as poly-(9,9-dioctyl-fluorenes-altogether-N-(4-butyl phenyl)-diphenylamines) ［ TFB ］ of hole transporting material (the 3rd composition) that the hole transporting layer of comparative example 2-1～comparative example 2-25 forms with ink.TFB contains pi-conjugated high molecular organic compound.Do not contain the aliphatic solvent as the 2nd composition.The 1st composition is the good solvent of the above-mentioned hole transporting material of conduct the 3rd composition more than solubilized 0.1wt%.
Because forming, the hole transporting layer of comparative example 2-1～comparative example 2-25 do not contain the 2nd composition that surface tension is little with ink, so bad to being formed with the wetting autgmentability of peristome 104a of hole injection layer 131.On the other hand, due to the TFB as macromolecule hole transporting material containing as the 3rd composition, so with use compared with low molecular hole transporting material situation, be difficult for causing the 3rd composition in drying under reduced pressure aggegation, separate out.Therefore, the thickness inequality of wetting extended defect, functional layer, luminous bad these 3 evaluation characteristics are " △ ".
(comparative example 2-26)～(comparative example 2-50)
As shown in figure 24, to form with ink be that cooperation is the diethylene glycol butyl methyl ether of 212 ℃ and makes it contain 0.5wt% to form as the TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of comparative example 2-26～comparative example 2-50.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 80vol%, and the volume ratio of the 2nd composition is 20vol%.The boiling point of the 1st composition is higher than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is 39 ℃～121 ℃.The dissolubility that the 1st composition and the 2nd composition compare the 3rd composition is high.In addition, the 2nd composition is less than the 1st component list surface tension.
(comparative example 2-51)～(comparative example 2-75)
As shown in figure 25, to form with ink be that cooperation is the dibutyl ethylene glycol ether of 256 ℃ and makes it contain 0.5wt% to form as the TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of comparative example 2-51～comparative example 2-75.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 80vol%, and the volume ratio of the 2nd composition is 20vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-5 ℃～77 ℃.The dissolubility that the 1st composition and the 2nd composition compare the 3rd composition is high.In addition, the 2nd composition is less than the 1st component list surface tension.
(comparative example 2-76)～(comparative example 2-100)
As shown in figure 26, to form with ink be that cooperation is the tetraethyleneglycol dimethyl ether of 275 ℃ and makes it contain 0.5wt% to form as the TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of comparative example 2-76～comparative example 2-100.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 80vol%, and the volume ratio of the 2nd composition is 20vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-24 ℃～58 ℃.The dissolubility that the 1st composition and the 2nd composition compare the 3rd composition is high.In addition, the 2nd composition is less than the 1st component list surface tension.
The hole transporting layer of comparative example 2-26～comparative example 2-100 forms surface tension 2nd composition less than the 1st composition that contains 20vol% with ink, but with the comparative example 1-1～comparative example 1-25 that does not contain the 2nd composition similarly, bad in the wetting autgmentability of peristome 104a.Thickness inequality, luminous bad these 3 the evaluation characteristics of wetting extended defect, functional layer are " △ ".
(embodiment 2-1)～(embodiment 2-25)
As shown in figure 27, to form with ink be that cooperation is the diethylene glycol butyl methyl ether of 212 ℃ and makes it contain 0.5wt% to form as the TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of embodiment 2-1～embodiment 2-25.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 70vol%, and the volume ratio of the 2nd composition is 30vol%.In other words, embodiment 2-1～embodiment 2-25 has increased 10vol% by the volume ratio of the 2nd composition for comparative example 2-26～comparative example 2-50.
The boiling point of the 1st composition poor Δ bp higher than the boiling point of the 2nd composition and its boiling point be 39 ℃～121 ℃ embodiment 2-1～embodiment 2-25 hole transporting layer form with ink by containing the 2nd composition of 30vol%, thereby improved the wetting autgmentability at peristome 104a compared with comparative example 2-26～comparative example 2-50.Wetting extended defect be evaluated as "○"～" ◎ ", the evaluation of thickness inequality is "○", luminous bad "○"～" ◎ " that be evaluated as.Particularly, the 3rd composition passes through to use high molecular TFB, thereby compared with using the situation of low molecular hole transporting material, has improved the evaluation characteristic not related with wetting extended defect, thickness.
(comparative example 2-101)～(comparative example 2-116) and (embodiment 2-26)～(embodiment 2-34)
As shown in figure 28, to form with ink be that cooperation is the dibutyl ethylene glycol ether of 256 ℃ and makes it contain 0.5wt% to form as the TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of comparative example 2-101～comparative example 2-116, embodiment 2-26～embodiment 2-34.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 70vol%, and the volume ratio of the 2nd composition is 30vol%.In other words, comparative example 2-101～comparative example 2-116 has increased 10vol% by the volume ratio of the 2nd composition for comparative example 2-51～comparative example 2-66.Embodiment 2-26～embodiment 2-34 has increased 10vol% by the volume ratio of the 2nd composition for comparative example 2-67～comparative example 2-75.
Although the hole transporting layer that the 1st composition and the poor Δ bp of the boiling point of the 2nd composition are comparative example 2-101～comparative example 2-116 of-5 ℃～26 ℃ forms surface tension 2nd composition less than the 1st composition that contains 30vol% with ink, but the wetting autgmentability at peristome 104a is bad, with comparative example 2-51～comparative example 2-66 similarly, 3 assessment items are " △ ".
On the other hand, the boiling point of the 1st composition poor Δ bp higher than the boiling point of the 2nd composition and its boiling point be 34 ℃～77 ℃ embodiment 2-26～embodiment 2-34 hole transporting layer form with ink by containing the 2nd composition of 30vol%, thereby compare in the wetting autgmentability of peristome 104a and improve with comparative example 2-101～comparative example 2-116 with comparative example 2-67～comparative example 2-75.The evaluation of wetting extended defect and thickness inequality is " ◎ ", luminous bad "○"～" ◎ " that be evaluated as.
(comparative example 2-117)～(comparative example 2-137) and (embodiment 2-35)～(embodiment 2-38)
As shown in figure 29, to form with ink be that cooperation is the tetraethyleneglycol dimethyl ether of 275 ℃ and makes it contain 0.5wt% to form as the TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of comparative example 2-117～comparative example 2-137, embodiment 2-35～embodiment 2-38.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 70vol%, and the volume ratio of the 2nd composition is 30vol%.In other words, comparative example 2-117～comparative example 2-137 has increased 10vol% by the volume ratio of the 2nd composition for comparative example 2-76～comparative example 2-96.Embodiment 2-35～embodiment 2-38 has increased 10vol% by the volume ratio of the 2nd composition for comparative example 2-97～comparative example 2-100.
Although the hole transporting layer that the 1st composition and the poor Δ bp of the boiling point of the 2nd composition are comparative example 2-117～comparative example 2-137 of-24 ℃～23 ℃ forms surface tension 2nd composition less than the 1st composition that contains 30vol% with ink, bad in the wetting autgmentability of peristome 104a.Especially the boiling point of the 1st composition than low-boiling comparative example 2-117～comparative example 2-125 of the 2nd composition in, the effect that contains the 2nd composition that surface tension is little is not almost brought into play, 3 assessment items are "×".In the wetting autgmentability of peristome 104a, along with the poor Δ bp of boiling point becomes the trend that presents greatly improvement, but 3 assessment items are " △ " in comparative example 2-126～comparative example 2-137.
On the other hand, the boiling point of the 1st composition poor Δ bp higher than the boiling point of the 2nd composition and boiling point is that the hole transporting layer of embodiment 2-35～embodiment 2-38 of 30 ℃～58 ℃ forms with ink by containing the 2nd composition of 30vol%, thereby improves with the wetting autgmentability that comparative example 2-97～comparative example 2-100 compares hole injection layer 131.Uneven and luminous bad "○"～" ◎ " that be evaluated as of wetting extended defect, thickness.
(embodiment 2-39)～(embodiment 2-63)
As shown in figure 30, the hole transporting layer of embodiment 2-39～embodiment 2-63 form with ink be using as each the 1st composition of above-mentioned 25 kinds of aromatic solvents and as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition be the diethylene glycol butyl methyl ether of 212 ℃ take volume ratio respectively as 50vol% coordinates, and make it contain that 0.5wt% forms as the TFB as hole transporting material of the 3rd composition.In other words, embodiment 2-39～embodiment 2-63 has increased 30vol% by the volume ratio of the 2nd composition for comparative example 2-26～comparative example 2-50.In other words, for embodiment 2-1～embodiment 2-25, the volume ratio of the 2nd composition has been increased to 10vol%.
The boiling point of the 1st composition poor Δ bp higher than the boiling point of the 2nd composition and boiling point be 39 ℃～121 ℃ embodiment 2-39～embodiment 2-63 hole transporting layer form with ink by surface tension 2nd composition less than the 1st composition that contains 50vol%, thereby improve in the wetting autgmentability of peristome 104a compared with comparative example 2-26～comparative example 2-50.In addition, by boiling point 2nd composition lower than the 1st composition that contains 50vol%, thereby compared with comparative example 2-26～comparative example 2-50, maintained hole transporting layer formation ink and be dried in the state of the wetting expansion of peristome 104a, the thickness inequality of hole transporting layer 132 also diminishes.Therefore, suppressed by luminous bad generations such as wetting extended defect, the uneven caused dim spot of thickness, bright spots.Therefore, wetting extended defect be evaluated as "○"～" ◎ ", thickness inequality be evaluated as "○", luminous bad be "○"～" ◎ ".
(comparative example 2-138)～(comparative example 2-153) and (embodiment 2-64)～(embodiment 2-72)
As shown in figure 31, the hole transporting layer of comparative example 2-138～comparative example 2-153 and embodiment 2-64～embodiment 2-72 form with ink be using as each the 1st composition of above-mentioned 25 kinds of aromatic solvents and the dibutyl ethylene glycol ether that is 256 ℃ as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition coordinate with volume ratio each 50%, and make it contain 0.3wt% forming as the high molecular TFB of hole transporting material as the 3rd composition.In comparative example 2-138 and comparative example 2-139, the boiling point of the 2nd composition is higher than the boiling point of the 1st composition, and the poor Δ bp of its boiling point is-5 ℃ ,-3 ℃.On the other hand, in comparative example 2-140～comparative example 2-153 and embodiment 2-64～embodiment 2-72, the boiling point of the 1st composition is higher than the boiling point of the 2nd composition, and the poor Δ bp of its boiling point is 2 ℃～77 ℃.The dissolubility that the 1st composition and the 2nd composition compare the 3rd composition is high.In addition, the 2nd composition is less than the 1st component list surface tension.
In the poor Δ bp of the boiling point of the 1st composition and the 2nd composition is less than comparative example 2-138～comparative example 2-153 of 30 ℃, by adding improving effect and still just cannot giving full play to of wetting autgmentability that surface tension 2nd composition less than the 1st composition produce.The wetting extended defect of comparative example 2-138～comparative example 2-153, thickness inequality, luminous bad these 3 evaluation characteristics are " △ ".
On the other hand, in embodiment 2-64～embodiment 2-72, significantly present by the improvement trend of adding the wetting autgmentability that poor Δ bp the 2nd composition above for 34 ℃ and that surface tension is less than the 1st composition of the 1st composition and the boiling point of the 2nd composition produces.The evaluation of wetting extended defect and thickness inequality is " ◎ ".Luminous bad evaluation is along with the value of the poor Δ bp of boiling point becomes large and becomes "○"～" ◎ ".
(comparative example 2-154)～(comparative example 2-174) and (embodiment 2-73)～(embodiment 2-76)
Shown in figure 32, the hole transporting layer of comparative example 2-154～comparative example 2-174 and embodiment 2-73～embodiment 2-76 form with ink be using as each the 1st composition of above-mentioned 25 kinds of aromatic solvents and as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition be the tetraethyleneglycol dimethyl ether of 275 ℃ take volume ratio respectively as 50% coordinates, and make it contain 0.5wt% forming as the high molecular TFB of hole transporting material as the 3rd composition.In comparative example 2-154～comparative example 2-165, the boiling point of the 2nd composition is higher than the boiling point of the 1st composition, and the poor Δ bp of its boiling point is-24 ℃ and-1 ℃.On the other hand, in comparative example 2-166～comparative example 2-174 and embodiment 2-73～embodiment 2-76, the boiling point of the 1st composition is higher than the boiling point of the 2nd composition, and the poor Δ bp of its boiling point is 0 ℃～58 ℃.The dissolubility that the 1st composition and the 2nd composition compare the 3rd composition is high.In addition, the 2nd composition is less than the 1st component list surface tension.
Be in the comparative example 2-154～comparative example 2-174 below 23 ℃ at the poor Δ bp of the boiling point of the 1st composition and the boiling point of the 2nd composition, even if the 2nd composition that the surface tension that contains 50vol% is less than the 1st composition, also can not get the capillary effect of the 2nd composition, not so good in the wetting autgmentability of peristome 104a.Particularly, in the boiling point of the 2nd composition comparative example 2-154～comparative example 2-162 higher than the boiling point of the 1st composition, wetting extended defect, thickness inequality, luminous bad each evaluation are "×".The wetting extended defect of comparative example 2-163～comparative example 2-174, thickness inequality, luminous bad each evaluation are " △ ".
On the other hand, in embodiment 2-73～embodiment 2-76, the poor Δ bp improvement trend above for 30 ℃ and the wetting autgmentability that surface tension 2nd composition less than the 1st composition produces of the boiling point by adding the 1st composition and the 2nd composition presents.Wetting extended defect, thickness inequality, luminous bad each evaluation are "○"～◎ along with the value of the poor Δ bp of boiling point becomes greatly ".When to select boiling point be the 2nd composition of 275 ℃, preferably select boiling point above to be 305 ℃ of the 1st compositions above than its high 30 ℃.
(embodiment 2-77)～(embodiment 2-101)
As shown in figure 33, to form with ink be that cooperation is the diethylene glycol butyl methyl ether of 212 ℃ and makes it contain 0.5wt% to form as the TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of embodiment 2-77～embodiment 2-101.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 30vol%, and the volume ratio of the 2nd composition is 70vol%.In other words, embodiment 2-77～embodiment 2-101 has increased 50vol% by the volume ratio of the 2nd composition for comparative example 2-26～comparative example 2-50.In other words, for embodiment 2-1～embodiment 2-25, the volume ratio of the 2nd composition has been increased to 40vol%.
The boiling point of the 1st composition poor Δ bp higher than the boiling point of the 2nd composition and boiling point is that the hole transporting layer of embodiment 2-77～embodiment 2-101 of 39 ℃～121 ℃ forms with ink by surface tension 2nd composition less than the 1st composition that contains 70vol%, thereby be presented at the stable wetting autgmentability of peristome 104a, wetting extended defect be evaluated as "○"～" ◎ ".The evaluation of thickness inequality is "○", luminous bad "○"～" ◎ " that be evaluated as.
(comparative example 2-175)～(comparative example 2-190) and (embodiment 2-102)～(embodiment 2-110)
As shown in figure 34, to form with ink be that cooperation is the dibutyl ethylene glycol ether of 256 ℃ and makes it contain 0.5wt% to form as the high molecular TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of comparative example 2-175～comparative example 2-190, embodiment 2-102～embodiment 2-110.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 30vol%, and the volume ratio of the 2nd composition is 70vol%.In other words, comparative example 2-175～comparative example 2-190 has increased 20vol% by the volume ratio of the 2nd composition for comparative example 2-138～comparative example 2-153.In addition, embodiment 2-102～embodiment 2-110 has increased 20vol% by the volume ratio of the 2nd composition for embodiment 2-64～embodiment 2-72.
In the poor Δ bp of the boiling point of the 1st composition and the 2nd composition is less than comparative example 2-175～comparative example 2-190 of 30 ℃, by adding improving effect and still just cannot giving full play to of wetting autgmentability that surface tension 2nd composition less than the 1st composition produce.The wetting extended defect of comparative example 2-175～comparative example 2-190, thickness inequality, luminous bad these 3 evaluation characteristics are " △ ".
On the other hand, in embodiment 2-102～embodiment 2-110, significantly present by the improvement trend of adding the wetting autgmentability that poor Δ bp the 2nd composition above for 34 ℃ and that surface tension is less than the 1st composition of the 1st composition and the boiling point of the 2nd composition produces.The evaluation of wetting extended defect and thickness inequality is " ◎ ".Luminous bad evaluation is along with the value of the poor Δ bp of boiling point becomes large and becomes "○"～" ◎ ".
(comparative example 2-191)～(comparative example 2-211) and (embodiment 2-111)～(embodiment 2-114)
As shown in figure 35, to form with ink be that cooperation is the tetraethyleneglycol dimethyl ether of 275 ℃ and makes it contain 0.5wt% to form as the high molecular TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of comparative example 2-191～comparative example 2-211, embodiment 2-111～embodiment 2-114.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 30vol%, and the volume ratio of the 2nd composition is 70vol%.In other words, comparative example 2-191～comparative example 2-211 has increased 20vol% by the volume ratio of the 2nd composition for comparative example 2-154～comparative example 2-174.Embodiment 2-111～embodiment 2-114 has increased 20vol% by the volume ratio of the 2nd composition for embodiment 2-73～embodiment 2-76.
Even surface tension 2nd composition less than the 1st composition that the boiling point of the 1st composition and the poor Δ bp of the boiling point of the 2nd composition are 23 ℃ of following comparative example 2-191～comparative example 2-211 contains 70vol%, the capillary effect that also can not get the 2nd composition is not so well in the wetting autgmentability of peristome 104a.Particularly, in the boiling point poor Δ bp higher than the boiling point of the 1st composition and its boiling point of the 2nd composition is comparative example 2-191～comparative example 2-199 of-24 ℃～-5 ℃, wetting extended defect, thickness inequality, luminous bad each evaluation characteristic are "×".The poor Δ bp of boiling point is that wetting extended defect, thickness inequality, the luminous bad each evaluation of comparative example 2-200～comparative example 2-211 of-3 ℃～23 ℃ is " △ ".
On the other hand, in the boiling point poor Δ bp higher than the boiling point of the 2nd composition and its boiling point of the 1st composition is embodiment 2-111～embodiment 2-114 of 30 ℃～58 ℃, significantly present by the improvement trend of adding the wetting autgmentability that surface tension the 2nd composition less than the 1st composition produce.Wetting extended defect, thickness inequality and luminous bad evaluation are respectively "○"～" ◎ ".
(comparative example 2-212)～(comparative example 2-236)
As shown in figure 36, to form with ink be that cooperation is the diethylene glycol butyl methyl ether of 212 ℃ and makes it contain 0.5wt% to form as the TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of comparative example 2-212～comparative example 2-236.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 20vol%, and the volume ratio of the 2nd composition is 80vol%.In other words, comparative example 2-212～comparative example 2-236 has increased 60vol% by the volume ratio of the 2nd composition for comparative example 2-26～comparative example 2-50.In other words, for embodiment 2-77～embodiment 2-101, the volume ratio of the 2nd composition has been increased to 10vol%.
The boiling point of the 1st composition poor Δ bp higher than the boiling point of the 2nd composition and its boiling point is that comparative example 2-212～comparative example 2-236 of 39 ℃～121 ℃ is by containing 80vol% the 2nd composition, thereby the excellent wetting autgmentability that is presented at peristome 104a, it is evaluated as "○"～" ◎ ".But, in drying under reduced pressure due to the evaporation of the 2nd composition finish after amount decline compared with embodiment 2-77～embodiment 2-101 of remaining the 1st composition, so obviously produce thickness inequality as the cohesion of the TFB as macromolecular material of the 3rd composition.Therefore, the uneven and luminous bad "×" that is evaluated as of thickness.
(comparative example 2-237)～(comparative example 2-261)
As shown in figure 37, to form with ink be that cooperation is the dibutyl ethylene glycol ether of 256 ℃ and makes it contain 0.5wt% to form as the high molecular TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of comparative example 2-237～comparative example 2-261.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 20vol%, and the volume ratio of the 2nd composition is 80vol%.In other words, comparative example 2-237～comparative example 2-261 has increased 60vol% by the volume ratio of the 2nd composition for comparative example 2-51～comparative example 2-75.In other words, for comparative example 2-175～comparative example 2-190 and embodiment 2-102～embodiment 2-110, the volume ratio of the 2nd composition has been increased to 10vol%.
Although the 2nd composition that comparative example 2-237～comparative example 2-252 that the poor Δ bp of the boiling point of the boiling point of the boiling point of the 1st composition and the 2nd composition is-5 ℃～26 ℃ contains 80vol%, bad in the wetting autgmentability of peristome 104a, its evaluation is " △ ".
The boiling point of the 1st composition poor Δ bp higher than the boiling point of the 2nd composition and its boiling point is that comparative example 2-253～comparative example 2-261 of 34 ℃～77 ℃ is by containing the 2nd composition of 80vol%, thereby the excellent wetting autgmentability that is presented at peristome 104a, its evaluation is " ◎ ".But, for comparative example 2-237～comparative example 2-261, due to the evaporation of the 2nd composition in drying under reduced pressure finish after amount decline compared with embodiment 2-102～embodiment 2-110 of remaining the 1st composition, so obviously produce thickness inequality as the cohesion of the TFB as macromolecular material of the 3rd composition.Therefore, the uneven and luminous bad "×" that is evaluated as of thickness.
(comparative example 2-262)～(comparative example 2-286)
As shown in figure 38, to form with ink be that cooperation is the tetraethyleneglycol dimethyl ether of 275 ℃ and makes it contain 0.5wt% to form as the high molecular TFB as hole transporting material of the 3rd composition as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to the hole transporting layer of comparative example 2-262～comparative example 2-286.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 20vol%, and the volume ratio of the 2nd composition is 80vol%.In other words, comparative example 2-262～comparative example 2-286 has increased 60vol% by the volume ratio of the 2nd composition for comparative example 2-76～comparative example 2-100.In other words, for comparative example 2-191～comparative example 2-211 and embodiment 2-111～embodiment 2-114, the volume ratio of the 2nd composition has been increased to 10vol%.
Although the 2nd composition that comparative example 2-262～comparative example 2-282 that the poor Δ bp of the boiling point of the boiling point of the boiling point of the 1st composition and the 2nd composition is-24 ℃～23 ℃ contains 80vol%, but the wetting autgmentability at peristome 104a is bad, its evaluation improves greatly along with the value change of the poor Δ bp of boiling point but still is "×"～" △ ".
The boiling point of the 1st composition poor Δ bp higher than the boiling point of the 2nd composition and its boiling point is that comparative example 2-283～comparative example 2-286 of 30 ℃～58 ℃ is by containing the 2nd composition of 80vol%, thereby the excellent wetting autgmentability that is presented at peristome 104a, it is evaluated as "○"～" ◎ ".But, for comparative example 2-262～comparative example 2-286, due to the evaporation of the 2nd composition in drying under reduced pressure finish after amount decline compared with embodiment 2-111～embodiment 2-114 of remaining the 1st composition, so obviously produce thickness inequality as the cohesion of the TFB as macromolecular material of the 3rd composition.Therefore, the uneven and luminous bad "×" that is evaluated as of thickness.
For the hole transporting layer formation ink of above-mentioned comparative example and embodiment, evaluation result is summarized as follows.
Hole transporting layer forms and contains the TFB as the high molecular hole transporting material of conduct of the 3rd composition with ink, is coated in the peristome 104a in next door 104 on hole injection layer 131.Do not contain as comparative example 2-1～comparative example 2-25 of the 2nd composition of aliphatic solvent bad in the wetting autgmentability of peristome 104a.In addition, in the comparative example 2-26～comparative example 2-100 that is 20vol% at the volume ratio of the 2nd composition, still bad in the wetting autgmentability of peristome 104a, thickness inequality and luminous bad evaluation are " △ ".In addition, in the comparative example 2-212～comparative example 2-286 that is 80vol% at the volume ratio of surface tension the 2nd composition less than the 1st composition, the poor Δ bp of the boiling point of the 1st composition and the 2nd composition is wetting favorable expandability when more than 30 ℃, if but that the poor Δ bp of boiling point is less than the boiling point of 30 ℃ or the 2nd composition is higher than the boiling point of the 1st composition, wetting autgmentability obviously declines.In comparative example 2-212～comparative example 2-286, all cannot form the hole transporting layer 132 with target film thickness.
On the other hand, in embodiment 2-1～embodiment 2-114, poor Δ bp higher than the boiling point of the 2nd composition according to the boiling point of the 1st composition and boiling point is that 30 ℃ of above modes are selected the 1st composition from 25 kinds of aromatic solvents, selects the 2nd composition from 3 kinds of aliphatic solvents.The volume ratio of the 2nd composition in the mixed solvent that in addition, contains the 1st composition and the 2nd composition is 30vol%～70vol%.Form the formation with the mixed solvent of ink by becoming such hole transporting layer, thereby while using high molecular hole transporting material as the 3rd composition, at the wetting resistant expansibility excellent of peristome 104a, after drying under reduced pressure, can form thickness inequality, luminous bad few hole transporting layer 132.
Comparative example 2-101～comparative example 2-211 and embodiment 2-1～embodiment 2-114 are similarly, the scope that the volume ratio that makes the 2nd composition in mixed solvent is 30vol%～70vol%, but when the 1st composition is less than 30 ℃ with the poor Δ bp of the boiling point of the 2nd composition or when the boiling point of the 2nd composition is higher than the boiling point of the 1st composition, wetting autgmentability declines compared with embodiment 2-1～embodiment 2-114.
< luminescent layer forms uses ink >
Figure 39 represents that luminescent layer forms the formation of the comparative example 3-1～comparative example 3-25 that uses ink and the table of evaluation result.Figure 40 represents that luminescent layer forms the formation of the comparative example 3-26～comparative example 3-50 that uses ink and the table of evaluation result.Figure 41 represents that luminescent layer forms the formation of the comparative example 3-51～comparative example 3-75 that uses ink and the table of evaluation result.Figure 42 represents that luminescent layer forms the formation of the comparative example 3-76～comparative example 3-100 that uses ink and the table of evaluation result.Figure 43 represents that luminescent layer forms the formation of the embodiment 3-1～embodiment 3-25 that uses ink and the table of evaluation result.Figure 44 represents that luminescent layer forms comparative example 3-101～comparative example 3-116 and the formation of embodiment 3-26～embodiment 3-34 and the table of evaluation result with ink.Figure 45 represents that luminescent layer forms comparative example 3-117～comparative example 3-137 and the formation of embodiment 3-35～embodiment 3-38 and the table of evaluation result with ink.Figure 46 represents that luminescent layer forms the formation of the embodiment 3-39～embodiment 3-63 that uses ink and the table of evaluation result.Figure 47 represents that luminescent layer forms comparative example 3-138～comparative example 3-153 and the formation of embodiment 3-64～embodiment 3-72 and the table of evaluation result with ink.Figure 48 represents that luminescent layer forms comparative example 3-154～comparative example 3-174 and the formation of embodiment 3-73～embodiment 3-76 and the table of evaluation result with ink.Figure 49 represents that luminescent layer forms the formation of the embodiment 3-77～embodiment 3-101 that uses ink and the table of evaluation result.Figure 50 represents that luminescent layer forms comparative example 3-175～comparative example 3-190 and the formation of embodiment 3-102～embodiment 3-110 and the table of evaluation result with ink.Figure 51 represents that luminescent layer forms comparative example 3-191～comparative example 3-211 and the formation of embodiment 3-111～embodiment 3-114 and the table of evaluation result with ink.Figure 52 represents that luminescent layer forms the formation of the comparative example 3-212～comparative example 3-236 that uses ink and the table of evaluation result.Figure 53 represents that luminescent layer forms the formation of the comparative example 3-237～comparative example 3-261 that uses ink and the table of evaluation result.Figure 54 represents that luminescent layer forms the formation of the comparative example 3-262～comparative example 3-286 that uses ink and the table of evaluation result.Should illustrate, in the table of Figure 39～Figure 54, as 25 kinds of aromatic solvents of the 1st composition to be recorded from the top mode that boiling point uprises successively downwards of table.
It is to select the 1st composition from above-mentioned 25 kinds of aromatic solvents with ink that the luminescent layer of comparative example 3-1～comparative example 3-286, embodiment 3-1～embodiment 3-114 forms, from 3 kinds of aliphatic solvents, select the 2nd composition, the volume ratio that changes each composition utilizes ink-jet method to form luminescent layer 133.Particularly, first, utilize liquid phase process (ink-jet method) to form hole injection layer 131 and hole transporting layer 132.,, use each luminescent layer of comparative example 3-1～comparative example 3-286, embodiment 3-1～embodiment 3-114 to form with ink formation luminescent layer 133 thereafter.Then, utilize vapour deposition method, form electron supplying layer 134, electron injecting layer 135.The material of each layer is constructed as follows.Hole injection layer 131 is m-MTDATA+TFB, and hole transporting layer 132 is TFB, and the material of main part of luminescent layer 133 is that TDAPB, dopant are Ir (ppy)
3, electron supplying layer 134 is BAlq, electron injecting layer 135 is LiF.
The luminescent layer of comparative example 3-1～comparative example 3-286, embodiment 3-1～embodiment 3-114 forms by the evaluation method of ink identical with the situation of above-mentioned hole injection layer formation ink, evaluates based on wetting extended defect, the inequality of thickness, luminous bad these 3 assessment items.Wherein, except evaluating forming the defect causing by the thickness inequality of the hole transporting layer 132 of ink by being coated with luminescent layer.Luminous bad evaluation too.
(comparative example 3-1)～(comparative example 3-25)
As shown in figure 39, it is that the luminescent layer formation material (the 3rd composition) that contains 0.5wt% in each the 1st composition making as above-mentioned 25 kinds of aromatic solvents forms that the luminescent layer of comparative example 3-1～comparative example 3-25 forms with ink, and it is to add the metal complex Ir (ppy) as the iridium of dopant in the TDAPB as material of main part that described luminescent layer forms material (the 3rd composition)
3form.In other words, the 3rd composition contains as containing the pi-conjugated TDAPB of low molecular organic compound and the metal complex of iridium.Do not contain the aliphatic solvent as the 2nd composition.The 1st composition is the good solvent that the above-mentioned luminescent layer of conduct the 3rd composition more than solubilized 0.1wt% forms material.
The luminescent layer of comparative example 3-1～comparative example 3-25 forms with ink owing to not containing the 2nd composition that surface tension is less than the 1st composition, so bad in the wetting autgmentability of peristome 104a that is formed with hole transporting layer 132.On the other hand, although contain as the low molecular above-mentioned luminescent layer of the 3rd composition and form material, but on the hole transporting layer 132 forming with liquid phase process, formation Film Thickness Ratio hole injection layer 131, (thick) luminescent layer 133 that hole transporting layer 132 is large, so the cohesion of the 3rd composition is difficult to produce.Therefore, the thickness inequality of wetting extended defect, luminescent layer 133, luminous bad these 3 evaluation characteristics are " △ ".
(comparative example 3-26)～(comparative example 3-50)
As shown in figure 40, to form with ink be to coordinate as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as above-mentioned 7 kinds of aliphatic solvent mid-boiling points of the 2nd composition to be the diethylene glycol butyl methyl ether of 212 ℃ and to make it contain 0.5wt% to form as the above-mentioned luminescent layer formation material of the 3rd composition to the luminescent layer of comparative example 3-26～comparative example 3-50.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 80vol%, and the volume ratio of the 2nd composition is 20vol%.The boiling point of the 1st composition is higher than the boiling point of the 2nd composition, and the poor Δ bp of its boiling point is 39 ℃～121 ℃.The 1st composition is to compare with the 2nd composition the good solvent that the dissolubility of the 3rd composition is high.In addition, the 2nd composition is less than the 1st component list surface tension.
(comparative example 3-51)～(comparative example 3-75)
As shown in figure 41, to form with ink be to coordinate as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to be the dibutyl ethylene glycol ether of 256 ℃ and to make it contain 0.5wt% to form as the above-mentioned luminescent layer formation material of the 3rd composition to the luminescent layer of comparative example 3-51～comparative example 3-75.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 80vol%, and the volume ratio of the 2nd composition is 20vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of its boiling point is-5 ℃～77 ℃.The 1st composition is to compare with the 2nd composition the good solvent that the dissolubility of the 3rd composition is high.In addition, the 2nd composition is less than the 1st component list surface tension.
(comparative example 3-76)～(comparative example 3-100)
As shown in figure 42, to form with ink be to coordinate as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to be the tetraethyleneglycol dimethyl ether of 275 ℃ and to make it contain 0.5wt% to form as the above-mentioned luminescent layer formation material of the 3rd composition to the luminescent layer of comparative example 3-76～comparative example 3-100.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 80vol%, and the volume ratio of the 2nd composition is 20vol%.The boiling point of the 1st composition is not necessarily high than the boiling point of the 2nd composition, and the poor Δ bp of boiling point is-24 ℃～58 ℃.The 1st composition is to compare with the 2nd composition the good solvent that the dissolubility of the 3rd composition is high.In addition, the 2nd composition is less than the 1st component list surface tension.
The luminescent layer of comparative example 3-26～comparative example 3-100 forms surface tension 2nd composition less than the 1st composition that contains 20vol% with ink, but with the comparative example 3-1～comparative example 3-25 that does not contain the 2nd composition similarly, bad in the wetting autgmentability of peristome 104a.Thickness inequality, luminous bad these 3 the evaluation characteristics of wetting extended defect, functional layer are " △ ".
(embodiment 3-1)～(embodiment 3-25)
As shown in figure 43, the formation of the luminescent layer of embodiment 3-1～embodiment 3-25 is to coordinate as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to be the diethylene glycol butyl methyl ether of 212 ℃ and to contain the TDAPB+Ir (ppy) as luminescent layer formation material of 0.5wt% as the 3rd composition with ink
3form.The volume ratio of the 1st composition is 70vol%, and the volume ratio of the 2nd composition is 30vol%.The boiling point of the 1st composition is higher than the boiling point of the 2nd composition, and the poor Δ bp of its boiling point is shown as 39 ℃～121 ℃.The dissolubility that the 1st composition and the 2nd composition compare the 3rd composition is high.In addition, the 2nd composition is less than the 1st component list surface tension.In other words, embodiment 3-1～embodiment 3-25 has increased 10vol% by the volume ratio of the 2nd composition for comparative example 3-26～comparative example 3-50.Should illustrate, the 3rd composition is not single component, contains as the TDAPB of material of main part with as the Ir (ppy) of dopant (guest materials)
3so, in the mixed solvent of the 1st composition and the 2nd composition more than solubilized 0.1wt%.
The luminescent layer of embodiment 3-1～embodiment 3-25 forms with ink by surface tension 2nd composition less than the 1st composition that contains 30vol%, thereby improves compared with comparative example 3-26～comparative example 3-50 in the wetting autgmentability of peristome 104a.In addition, by boiling point 2nd composition lower than the 1st composition that contains 30vol%, thereby compared with comparative example 3-26～comparative example 3-50, in drying under reduced pressure, maintain luminescent layer and formed the state in the wetting expansion of peristome 104a with ink, and promote to be dried, the thickness inequality of luminescent layer 133 also diminishes.Therefore, suppressed by luminous bad generations such as wetting extended defect, the uneven caused dim spot of thickness, bright spots.Particularly, owing to being coated with luminescent layer formation ink on the hole transporting layer 132 forming with liquid phase process, so wetting resistant expansibility excellent.Therefore, wetting extended defect is " ◎ ", and the thickness of luminescent layer is not "○", luminous bad be " ◎ ".
(comparative example 3-101)～(comparative example 3-116) and (embodiment 3-26)～(embodiment 3-34)
As shown in figure 44, the formation of the luminescent layer of comparative example 3-101～comparative example 3-116 and embodiment 3-26～embodiment 3-34 is to coordinate as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to be the dibutyl ethylene glycol ether of 256 ℃ and to contain the TDAPB+Ir (ppy) as luminescent layer formation material of 0.5wt% as the 3rd composition with ink
3form.The volume ratio of the 1st composition is 70vol%, and the volume ratio of the 2nd composition is 30vol%.In comparative example 3-101 and comparative example 3-102, the boiling point of the 2nd composition is higher than the boiling point of the 1st composition, and its poor Δ bp is-5 ℃ ,-3 ℃.On the other hand, in comparative example 3-103～comparative example 3-116 and embodiment 3-26～embodiment 3-34, the boiling point of the 1st composition is higher than the boiling point of the 2nd composition, and the poor Δ bp of its boiling point is shown as 2 ℃～77 ℃.The 1st composition is to compare with the 2nd composition the good solvent that the dissolubility of the 3rd composition is high.In addition, the 2nd composition is less than the 1st component list surface tension.The 3rd composition that contains as mentioned above multiple material is in the mixed solvent that contains the 1st composition and the 2nd composition more than solubilized 0.1wt%.
In the poor Δ bp of the boiling point of the 1st composition and the 2nd composition is less than comparative example 3-101～comparative example 3-116 of 30 ℃, by adding improving effect and still just cannot giving full play to of wetting autgmentability that surface tension 2nd composition less than the 1st composition produce.The wetting extended defect of comparative example 3-26～comparative example 3-41, thickness inequality, luminous bad these 3 evaluation characteristics are " △ ".
In embodiment 3-26～embodiment 3-34, present by the improvement trend of adding the wetting autgmentability that poor Δ bp the 2nd composition above for 30 ℃ and that surface tension is less than the 1st composition of the 1st composition and the boiling point of the 2nd composition produces.Wetting extended defect, thickness inequality and luminous bad evaluation characteristic become "○"～" ◎ ".
(comparative example 3-117)～(comparative example 3-137) and (embodiment 3-35)～(embodiment 3-38)
As shown in figure 45, the formation of the luminescent layer of comparative example 3-117～comparative example 3-137 and embodiment 3-35～embodiment 3-38 is to coordinate as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to be the tetraethyleneglycol dimethyl ether of 275 ℃ and to contain the TDAPB+Ir (ppy) as luminescent layer formation material of 0.5wt% as the 3rd composition with ink
3form.The volume ratio of the 1st composition is 70vol%, and the volume ratio of the 2nd composition is 30vol%.In comparative example 3-117～comparative example 3-128, the boiling point of the 2nd composition is higher than the boiling point of the 1st composition, and the poor Δ bp of its boiling point is-24 ℃ and-1 ℃.On the other hand, in comparative example 3-129～comparative example 3-137 and embodiment 3-35～embodiment 3-38, the boiling point of the 2nd composition equates with the boiling point of the 1st composition or is lower than it, and the poor Δ bp of its boiling point is shown as 0 ℃～58 ℃.The 1st composition is to compare with the 2nd composition the good solvent that the dissolubility of the 3rd composition is high.In addition, the 2nd composition is less than the 1st component list surface tension.The 3rd composition that contains as mentioned above multiple material is in the mixed solvent that contains the 1st composition and the 2nd composition more than solubilized 0.1wt%.
Be in the comparative example 3-117～comparative example 3-137 below 23 ℃ at the poor Δ bp of the boiling point of the 1st composition and the boiling point of the 2nd composition, even the 2nd composition that the surface tension that contains 30vol% is less than the 1st composition, also can not get the capillary effect of the 2nd composition, not so good in the wetting autgmentability of peristome 104a.Particularly, in the boiling point of the 2nd composition comparative example 3-117～comparative example 3-125 higher than the boiling point of the 1st composition, wetting extended defect, thickness inequality, luminous bad each evaluation characteristic are "×".The wetting extended defect of comparative example 3-126～comparative example 3-137, thickness inequality, luminous bad each evaluation characteristic are " △ ".
In embodiment 3-35～embodiment 3-38, present by the improvement trend of adding the wetting autgmentability that poor Δ bp the 2nd composition above for 30 ℃ and that surface tension is less than the 1st composition of the 1st composition and the boiling point of the 2nd composition produces.Wetting extended defect, thickness inequality, luminous bad each evaluation characteristic are "○"～" ◎ ".When to select boiling point be the 2nd composition of 275 ℃, preferably select boiling point to be above 305 ℃ of the 1st compositions above than its high 30 ℃.
(embodiment 3-39)～(embodiment 3-63)
The luminescent layer of embodiment 3-39～embodiment 3-63 of Figure 46 form with ink be using as each the 1st composition of above-mentioned 25 kinds of aromatic solvents and as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition be the diethylene glycol butyl methyl ether of 212 ℃ take volume ratio respectively as 50vol% coordinates, and make it contain the TDAPB+Ir (ppy) as luminescent layer formation material of 0.5wt% as the 3rd composition
3form.In other words, embodiment 3-39～embodiment 3-63 has increased 30vol% by the volume ratio of the 2nd composition for comparative example 3-26～comparative example 3-50.In other words, for embodiment 3-1～embodiment 3-25, the volume ratio of the 2nd composition has been increased to 20vol%.
The luminescent layer formation of embodiment 3-39～embodiment 3-63 similarly shows good wetting autgmentability at peristome 104a with ink and embodiment 3-1～embodiment 3-25, even if be also difficult for producing thickness inequality in drying under reduced pressure, soak be evaluated as " ◎ " of extended defect, thickness inequality be evaluated as "○", luminous bad being evaluated as " ◎ ".
(comparative example 3-138)～(comparative example 3-153) and (embodiment 3-64)～(embodiment 3-72)
As shown in figure 47, the luminescent layer of comparative example 3-138～comparative example 3-153 and embodiment 3-64～embodiment 3-72 form with ink be using as each the 1st composition of above-mentioned 25 kinds of aromatic solvents and as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition be the dibutyl ethylene glycol ether of 256 ℃ take volume ratio respectively as 50vol% coordinates, and make it contain the TDAPB+Ir (ppy) as luminescent layer formation material of 0.5wt% as the 3rd composition
3form.In other words, comparative example 3-138～comparative example 3-153 and embodiment 3-64～embodiment 3-72 have increased 20vol% by the volume ratio of the 2nd composition for comparative example 3-101～comparative example 3-116 and embodiment 3-26～embodiment 3-34.
In the poor Δ bp of the boiling point of the 1st composition and the boiling point of the 2nd composition is less than comparative example 3-138～comparative example 3-153 of 30 ℃, the effect of the wetting autgmentability of improvement producing by surface tension the 2nd composition less than the 1st composition that contains 50vol% is insufficient, but the effect of improving that is wetting autgmentability in more than 30 ℃ embodiment 3-64～embodiment 3-72 at the poor Δ bp of boiling point is brought into play.
Wetting extended defect, thickness inequality and the luminous bad evaluation of comparative example 3-138～comparative example 3-153 are " △ ".On the other hand, the wetting extended defect of embodiment 3-64～embodiment 3-72, thickness inequality and luminous bad evaluation are "○"～" ◎ ".
(comparative example 3-154)～(comparative example 3-174) and (embodiment 3-73)～(embodiment 3-76)
As shown in figure 48, the luminescent layer of comparative example 3-154～comparative example 3-174 and embodiment 3-73～embodiment 3-76 form with ink be using as each the 1st composition of above-mentioned 25 kinds of aromatic solvents and as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition be the tetraethyleneglycol dimethyl ether of 275 ℃ take volume ratio respectively as 50vol% coordinates, and contain the TDAPB+Ir (ppy) as luminescent layer formation material of 0.5wt% as the 3rd composition
3form.In other words, comparative example 3-154～comparative example 3-174 and embodiment 3-73～embodiment 3-76 have increased 20vol% by the volume ratio of the 2nd composition for comparative example 3-117～comparative example 3-137 and embodiment 3-35～embodiment 3-38.
In the poor Δ bp of the boiling point of the 1st composition and the boiling point of the 2nd composition is less than comparative example 3-154～comparative example 3-174 of 30 ℃, the effect of the wetting autgmentability of the caused improvement of the 2nd composition that surface tension by containing 50vol% is less than the 1st composition is still just insufficient.The effect of improving that is wetting autgmentability in more than 30 ℃ embodiment 3-73～embodiment 3-76 at the poor Δ bp of boiling point is brought into play.
The poor Δ bp of boiling point is that wetting extended defect, thickness inequality and the luminous bad evaluation of comparative example 3-154～comparative example 3-162 of-24 ℃～-5 ℃ is "×".The poor Δ bp of boiling point is that wetting extended defect, thickness inequality and the luminous bad evaluation of comparative example 3-163～comparative example 3-174 of-3 ℃～23 ℃ is " △ ".On the other hand, the wetting extended defect of embodiment 3-73～embodiment 3-76, thickness inequality and luminous bad evaluation are "○"～" ◎ ".
(embodiment 3-77)～(embodiment 3-101)
As shown in figure 49, the formation of the luminescent layer of embodiment 3-77～embodiment 3-101 is to coordinate as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to be the diethylene glycol butyl methyl ether of 212 ℃ and to contain the TDAPB+Ir (ppy) as luminescent layer formation material of 0.5wt% as the 3rd composition with ink
3form.The volume ratio of the 1st composition is 30vol%, and the volume ratio of the 2nd composition is 70vol%.In other words, embodiment 3-77～embodiment 3-101 has increased 20vol% by the volume ratio of the 2nd composition for embodiment 3-39～embodiment 3-63.
The luminescent layer formation of embodiment 3-77～embodiment 3-101 similarly shows good wetting autgmentability at peristome 104a with ink and embodiment 3-39～embodiment 3-63, even if be also difficult for producing thickness inequality in drying under reduced pressure, soak be evaluated as " ◎ " of extended defect, thickness inequality be evaluated as "○", luminous bad being evaluated as " ◎ ".
(comparative example 3-175)～(comparative example 3-190) and (embodiment 3-102)～(embodiment 3-110)
As shown in figure 50, the formation of the luminescent layer of comparative example 3-175～comparative example 3-190 and embodiment 3-102～embodiment 3-110 is to coordinate as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to be the dibutyl ethylene glycol ether of 256 ℃ and to contain the TDAPB+Ir (ppy) as luminescent layer formation material of 0.5wt% as the 3rd composition with ink
3form.The volume ratio of the 1st composition is 30vol%, and the volume ratio of the 2nd composition is 70vol%.In other words, comparative example 3-175～comparative example 3-190 and embodiment 3-102～embodiment 3-110 have increased 20vol% by the volume ratio of the 2nd composition for comparative example 3-138～comparative example 3-153 and embodiment 3-64～embodiment 3-72.
In the poor Δ bp of the boiling point of the 1st composition and the boiling point of the 2nd composition is less than comparative example 3-175～comparative example 3-190 of 30 ℃, the effect of the wetting autgmentability of improvement of bringing by surface tension the 2nd composition less than the 1st composition that contains 70vol% is insufficient, but the effect of improving that is wetting autgmentability in more than 30 ℃ embodiment 3-102～embodiment 3-110 at the poor Δ bp of boiling point is brought into play.
Wetting extended defect, thickness inequality and the luminous bad evaluation of comparative example 3-175～comparative example 3-190 are " △ ".On the other hand, the wetting extended defect of embodiment 3-102～embodiment 3-110, thickness inequality and luminous bad evaluation are "○"～" ◎ ".Particularly, in embodiment 3-103～embodiment 3-106,3 assessment items are " ◎ ", thereby preferably.
(comparative example 3-191)～(comparative example 3-211) and (embodiment 3-111)～(embodiment 3-114)
As shown in Figure 51, it is to coordinate as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to be the tetraethyleneglycol dimethyl ether of 275 ℃ and to contain the TDAPB+Ir (ppy) as luminescent layer formation material of 0.5wt% as the 3rd composition that the luminescent layer of comparative example 3-191～comparative example 3-211 and embodiment 3-111～embodiment 3-114 forms with ink
3form.The volume ratio of the 1st composition is 30vol%, and the volume ratio of the 2nd composition is 70vol%.In other words, comparative example 3-191～comparative example 3-211 and embodiment 3-111～embodiment 3-114 have increased 20vol% by the volume ratio of the 2nd composition for comparative example 3-154～comparative example 3-174 and embodiment 3-73～embodiment 3-76.
In the poor Δ bp of the boiling point of the 1st composition and the boiling point of the 2nd composition is less than comparative example 3-191～comparative example 3-211 of 30 ℃, the effect of the wetting autgmentability of improvement of bringing by surface tension the 2nd composition less than the 1st composition that contains 70vol% is still just insufficient.But the effect of improving that is wetting autgmentability in more than 30 ℃ embodiment 3-111～embodiment 3-114 at the poor Δ bp of boiling point is brought into play.
The poor Δ bp of boiling point is that wetting extended defect, thickness inequality and the luminous bad evaluation of comparative example 3-191～comparative example 3-199 of-24 ℃～-5 ℃ is "×".The poor Δ bp of boiling point is that wetting extended defect, thickness inequality and the luminous bad evaluation of comparative example 3-200～comparative example 3-211 of-3 ℃～23 ℃ is " △ ".On the other hand, being evaluated as of the wetting extended defect of embodiment 3-111～embodiment 3-114 " ◎ ", thickness inequality be evaluated as "○", luminous bad being evaluated as " ◎ ".
(comparative example 3-212)～(comparative example 3-236)
As shown in Figure 52, it is to coordinate as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to be the diethylene glycol butyl methyl ether of 212 ℃ and to contain 0.5wt% and form as the above-mentioned luminescent layer formation material of the 3rd composition that the luminescent layer of comparative example 3-212～comparative example 3-236 forms with ink.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 20vol%, and the volume ratio of the 2nd composition is 80vol%.In other words, for embodiment 3-77～embodiment 3-101, the volume ratio of the 2nd composition has been increased to 10vol%.
The boiling point of the 1st composition poor Δ bp higher than the boiling point of the 2nd composition and its boiling point is that comparative example 3-212～comparative example 3-236 of 39 ℃～121 ℃ is by containing the 2nd composition of 80vol%, thereby the excellent wetting autgmentability that is presented at peristome 104a, it is evaluated as " ◎ ".But, due to the evaporation of the 2nd composition in drying under reduced pressure finish after amount decline compared with embodiment 3-77～embodiment 3-101 of remaining the 1st composition, so as the luminescent layer containing low molecular material of the 3rd composition form material cohesion, separate out to become and significantly produce thickness inequality.Therefore, the uneven and luminous bad "×" that is evaluated as of thickness.
(comparative example 3-237)～(comparative example 3-261)
As shown in Figure 53, to form with ink be to coordinate as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to be the dibutyl ethylene glycol ether of 256 ℃ and to make it contain 0.5wt% to form as the above-mentioned luminescent layer formation material of the 3rd composition to the luminescent layer of comparative example 3-237～comparative example 3-261.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 20vol%, and the volume ratio of the 2nd composition is 80vol%.In other words, comparative example 3-237～comparative example 3-261 has increased 10vol% by the volume ratio of the 2nd composition for comparative example 3-175～comparative example 3-190 and embodiment 3-102～embodiment 3-110.
Although the 2nd composition that comparative example 3-237～comparative example 3-252 that the poor Δ bp of the boiling point of the boiling point of the boiling point of the 1st composition and the 2nd composition is-5 ℃～26 ℃ contains 80vol%, bad in the wetting autgmentability of peristome 104a, its evaluation is " △ ".
The boiling point of the 1st composition poor Δ bp higher than the boiling point of the 2nd composition and its boiling point is that comparative example 3-253～comparative example 3-261 of 34 ℃～77 ℃ is by containing the 2nd composition of 80vol%, thereby the excellent wetting autgmentability that is presented at peristome 104a, it is evaluated as "○"～" ◎ ".But, for comparative example 3-237～comparative example 3-261, due to the evaporation of the 2nd composition in drying under reduced pressure finish after amount decline compared with embodiment 3-102～embodiment 3-110 of remaining the 1st composition, so form with the cohesion of material, separate out and become significantly and generation thickness inequality as the luminescent layer containing low molecular material of the 3rd composition.Therefore, the uneven and luminous bad "×" that is evaluated as of thickness.
(comparative example 3-262)～(comparative example 3-286)
As shown in Figure 54, to form with ink be to coordinate as each the 1st composition of above-mentioned 25 kinds of aromatic solvents with as 7 kinds of aliphatic solvent mid-boiling points of above-mentioned the 2nd composition to be the tetraethyleneglycol dimethyl ether of 275 ℃ and to contain 0.5wt% and form as the above-mentioned luminescent layer formation material of the 3rd composition to the luminescent layer of comparative example 3-262～comparative example 3-286.The volume ratio of the 1st composition in the mixed solvent that contains the 1st composition and the 2nd composition is 20vol%, and the volume ratio of the 2nd composition is 80vol%.In other words, comparative example 3-262～comparative example 3-286 has increased 10vol% by the volume ratio of the 2nd composition for comparative example 3-191～comparative example 3-211 and embodiment 3-111～embodiment 3-114.
In the poor Δ bp of the boiling point of the 1st composition and the boiling point of the 2nd composition is less than comparative example 3-262～comparative example 3-282 of 30 ℃, the effect of the wetting autgmentability of the improvement that produces by surface tension the 2nd composition less than the 1st composition that contains 80vol% is still just insufficient, wetting extended defect be evaluated as "×"～" △ ".On the other hand, the effect of improving that is wetting autgmentability in more than 30 ℃ comparative example 3-283～comparative example 3-286 at the poor Δ bp of boiling point is brought into play, and soaks be evaluated as " ◎ " of extended defect.
But, for comparative example 3-262～comparative example 3-286, due to the evaporation of the 2nd composition in drying under reduced pressure finish after amount decline compared with embodiment 3-111～embodiment 3-114 of remaining the 1st composition, so form with the cohesion of material, separate out and become significantly and generation thickness inequality as the luminescent layer containing low molecular material of the 3rd composition.Therefore, the uneven and luminous bad "×" that is evaluated as of thickness.
For the luminescent layer formation ink of above-mentioned comparative example and embodiment, evaluation is summarized as follows.
Luminescent layer forms and contains low molecular luminescent layer with ink and form with material as the 3rd composition, is coated in the peristome 104a in next door 104 on hole transporting layer 132.Do not contain as comparative example 3-1～comparative example 3-25 of the 2nd composition of aliphatic solvent bad in the wetting autgmentability of peristome 104a.In addition, the wetting autgmentability of the comparative example 3-26～comparative example 3-100 split shed 104a of portion that is 20vol% at the volume ratio of the 2nd composition is also bad, and thickness inequality and luminous bad evaluation are " △ ".In addition, in the comparative example 3-212～comparative example 3-286 that is 80vol% at the volume ratio of surface tension the 2nd composition less than the 1st composition, the poor Δ bp of the boiling point of the 1st composition and the 2nd composition is wetting favorable expandability when more than 30 ℃, but the poor Δ bp of boiling point is less than the boiling point of 30 ℃ or the 2nd composition when higher than the boiling point of the 1st composition, and wetting autgmentability obviously reduces.In comparative example 3-212～comparative example 3-286, thickness is uneven to be produced, and all cannot form the luminescent layer 133 that luminous bad generation is few.
On the other hand, in embodiment 3-1～embodiment 3-114, poor Δ bp higher than the boiling point of the 1st composition according to the boiling point of the 2nd composition and boiling point is that 30 ℃ of above modes are selected the 1st composition from 25 kinds of aromatic solvents, selects the 2nd composition from 3 kinds of aliphatic solvents.The volume ratio of the 2nd composition in the mixed solvent that in addition, contains the 1st composition and the 2nd composition is 30vol%～70vol%.Form the formation with the mixed solvent of ink by becoming such luminescent layer, thereby while using low molecular luminescent layer to form material as the 3rd composition, at the wetting resistant expansibility excellent of peristome 104a, can be formed in drying under reduced pressure caudacoria thickness ununiformity, luminous bad few luminescent layer 133.
Comparative example 3-101～comparative example 3-211 and embodiment 3-1～embodiment 3-114 are similarly, the scope that the volume ratio that makes the 2nd composition in mixed solvent is 30vol%～70vol%, but when the 1st composition is less than 30 ℃ with the poor Δ bp of the boiling point of the 2nd composition or when the boiling point of the 2nd composition is higher than the boiling point of the 1st composition, wetting autgmentability reduces compared with embodiment 3-1～embodiment 3-114.
The effect of above-mentioned the 1st execution mode is as follows.
(1) hole injection layer of embodiment 1-1～embodiment 1-114 forms and contains a kind with ink to be selected from boiling point be that to be selected from boiling point be 200 ℃ of the 2nd compositions in 7 kinds of above aliphatic solvents and the 3rd composition as low molecular hole-injecting material for the 1st composition in 25 kinds of aromatic solvents of 250 ℃～350 ℃, a kind, the dissolubility of the 3rd composition is that the 1st composition is higher than the 2nd composition, the volume ratio of the 2nd composition in mixed solvent is 30vol%～70vol%, and the difference of the boiling point of the boiling point of the 1st composition and the 2nd composition is more than 30 ℃.Therefore, obtained using surface tension than the little aliphatic solvent of the aromatic solvent of the 1st composition the effect as the 2nd composition, if the hole injection layer at the peristome 104a coating the present embodiment being impaled by next door 104 forms with ink, can be in the wetting expansion of the peristome 104a that disposes pixel electrode 102, and to form dry caudacoria thickness ununiformity be ± 5% with interior hole injection layer 131 with respect to average film thickness.
(2) hole transporting layer of embodiment 2-1～embodiment 2-114 forms and contains a kind with ink to be selected from boiling point be that to be selected from boiling point be 200 ℃ of the 2nd compositions in 7 kinds of above aliphatic solvents and the 3rd composition as high molecular hole transporting material for the 1st composition in 25 kinds of aromatic solvents of 250 ℃～350 ℃, a kind, the dissolubility of the 3rd composition is that the 1st composition is higher than the 2nd composition, the volume ratio of the 2nd composition in mixed solvent is 30vol%～70vol%, and the difference of the boiling point of the boiling point of the 1st composition and the 2nd composition is more than 30 ℃.Therefore, obtained using surface tension than the little aliphatic solvent of the aromatic solvent of the 1st composition the effect as the 2nd composition, if the hole transporting layer at the peristome 104a coating the present embodiment being impaled by next door 104 forms with ink, can be in the wetting expansion of the peristome 104a that disposes the hole injection layer 131 forming with liquid phase process, and to form dry caudacoria thickness ununiformity be ± 2.5% with interior hole transporting layer 132 with respect to average film thickness.
(3) luminescent layer of embodiment 3-1～embodiment 3-114 forms and contains a kind with ink to be selected from boiling point be that to be selected from boiling point be 200 ℃ of the 2nd compositions in 7 kinds of above aliphatic solvents and the 3rd composition that forms material as low molecular luminescent layer for the 1st composition in 25 kinds of aromatic solvents of 250 ℃～350 ℃, a kind, the dissolubility of the 3rd composition is that the 1st composition is higher than the 2nd composition, the volume ratio of the 2nd composition is 30vol%～70vol%, and the difference of the boiling point of the boiling point of the 1st composition and the 2nd composition is more than 30 ℃.Therefore, obtained using surface tension than the little aliphatic solvent of the aromatic solvent of the 1st composition the effect as the 2nd composition, if the luminescent layer at the peristome 104a coating the present embodiment being impaled by next door 104 forms with ink, can be in the wetting expansion of the peristome 104a that disposes the hole transporting layer 132 forming with liquid phase process, and to form dry caudacoria thickness ununiformity be ± 2.5% with interior luminescent layer 133 with respect to average film thickness.
(4) form with for ink for the each functional layer of embodiment 1-1～embodiment 1-114, embodiment 2-1～embodiment 2-114, embodiment 3-1～embodiment 3-114, because the boiling point of the mixed solvent that contains the 1st composition and the 2nd composition is more than 200 ℃, so be difficult for the obstruction of the nozzle 21 that produces shower nozzle 20, obtain stable ejection characteristic, be therefore suitable for ink-jet method (drop ejection method).
(5) if use possess the present embodiment of being filled with functional layer form with ink as the ink tank 14 of ink reservoir or the blowoff 1 of print cartridge 140, can stably spray to the position (the peristome 104a in next door 104) of the upper regulation of the substrate W as target functional layer the formations ink of ormal weight, suppress the caused thickness inequality of crawling (wetting expansion) and form stable membranaceous functional layer.
(6), according to the manufacture method of the organic EL 130 of present embodiment, use the functional layer of present embodiment to form and utilize ink-jet method to form at least 1 layer in hole injection layer 131 in the functional layer 136 of organic EL 130, hole transporting layer 132, luminescent layer 133 with ink.Therefore, obtain stable membranaceous functional layer 136, so can rate of finished products manufacture well the organic EL 130 that obtains the desirable characteristics of luminescence (brightness, luminescent lifetime).And, the light-emitting device 100 that possesses this organic EL 130 can be provided.
Should illustrate, form with ink, above-mentioned hole transporting layer and form and form with in each embodiment of ink with ink, above-mentioned luminescent layer at above-mentioned hole injection layer, having selected boiling point is that the aromatic solvent of 250 ℃～350 ℃ is as the 1st composition.On the other hand, in the drying under reduced pressure operation of each ink, boiling point is lower and be the first start vaporizer of the 2nd composition of aliphatic solvent than the 1st composition, also remains the 1st composition after the evaporation of the 2nd composition finishes.Therefore, under identical drying under reduced pressure condition, because the boiling point of the 1st composition is higher, drying time is longer, if so consider the productivity ratio (drying time, drying under reduced pressure condition etc.) in drying under reduced pressure operation, preferably selecting boiling point is that 300 ℃ of following aromatic solvents are as the 1st composition.
The 2nd execution mode
Electronic equipment
Next, with reference to Figure 55, the electronic equipment of present embodiment is described.Figure 55 (a) is the schematic diagram representing as the notebook-PC of an example of electronic equipment, and Figure 55 (b) is the schematic diagram representing as the panel TV (TV) of an example of electronic equipment.
As shown in Figure 55 (a), personal computer 1000 as electronic equipment is made up of with the display unit 1003 that possesses display part 1004 main part 1001 that possesses keyboard 1002, and display unit 1003 is situated between by articulated structure portion rotatably support in main part 1001.
In this personal computer 1000, be equipped with the light-emitting device 100 of above-mentioned the 1st execution mode at display part 1004.
As shown in Figure 55 (b), be equipped with the light-emitting device 100 of above-mentioned the 1st execution mode at display part 1101 as panel TV (TV) 1100 of electronic equipment.
Be located at the organic EL 130 in sub-pixel 110R, 110G, the 110B of light-emitting device 100, use the functional layer of above-mentioned the 1st execution mode to form and utilize liquid phase process (ink-jet method) to form at least 1 layer in hole injection layer 131 in functional layer 136, hole transporting layer 132, luminescent layer 133 with ink.Therefore,, because thickness is uneven few, dim spot, bright spot etc. are luminous bad also few, so can rate of finished products manufacture well light-emitting device 100.In other words, can provide the personal computer 1000 of cost excellence, dull and stereotyped TV1100.
The electronic equipment that carries light-emitting device 100 is not limited to above-mentioned personal computer 1000, dull and stereotyped TV1100.For example, the video tape recorder that can enumerate the portable data assistance such as smart mobile phone, POS, guider, browser, digital camera, monitor direct viewing type etc. has the electronic equipment of display part.
The present invention is not limited to above-mentioned execution mode, can in the scope of not violating the inventive concept that obtains or thought from technical scheme and specification are all, suitably change, follow the functional layer of this change form by the manufacture method of ink, organic EL and use the light-emitting device of this organic EL, electronic equipment to be also included in technical scope of the present invention.Except above-mentioned execution mode, also consider various variation.Below, enumerating variation describes.
The functional layer formation of above-mentioned the 1st execution mode is not limited to a kind with the aromatic solvent in the 1st composition of ink, can become the formation that contains multiple aromatic solvent.Thus, can more easily adjust the dissolubility to the 3rd composition compared with the situation of a kind for example.
The functional layer formation of above-mentioned the 1st execution mode is not limited to a kind with the aliphatic solvent in the 2nd composition of ink, can become the formation that contains multiple aliphatic solvent.Thus, can easier adjustment form surface tension compared with the situation of a kind for example.
The functional layer formation of above-mentioned the 1st execution mode is not limited to contain a kind of functional material with the 3rd composition in ink, can contain several functions material.For example, can become and contain low molecule hole transporting material and the macromolecule hole transporting material formation as hole transporting material.Can improve thus cavity conveying.In addition, for example, in luminescent layer formation material, for each material of main part and dopant, can contain multiple material of main part or dopant.Can improve luminosity, life-span thus.
Variation 4
The functional layer of above-mentioned the 1st execution mode forms the material that is not limited to the functional layer 136 that forms organic EL 130 with the 3rd composition in ink.For example, if use organic semiconductor compound as the 3rd composition, can form semiconductor layer, the electrode etc. as the functional layer in thin-film transistor.In addition for example, also can form the function element such as electronics release portion in photoelectric conversion layer, FED (Field Emission Display), the SED (Surface-conduction-electron Emitter Display) of dye-sensitized solar cell.
The formation of the light-emitting device 100 of above-mentioned the 1st execution mode is not limited to have sub-pixel 110R, the 110G, the 110B that obtain different illuminant colours.Can possess redness (R), green (G), blue (B) for example sub-pixel of yellow (Y) in addition.In addition, be also not limited to carry out the formation of full-color demonstration, also can become and possess the formation that obtains monochromatic luminous organic EL 130.Thus, not only as display device, also can be provided as the light-emitting device 100 of lighting device.
Symbol description
1 ... blowoff, 14 ... as the ink tank of ink reservoir, 20 ... shower nozzle, 21 ... nozzle, 50 ... form the hole injection layer formation ink with ink as functional layer, 60 ... form the hole transporting layer formation ink with ink as functional layer, 70 ... form the luminescent layer formation ink with ink as functional layer, 100 ... light-emitting device, 101 ... device substrate, 102 ... as the pixel electrode of anode, 103 ... as the opposite electrode of negative electrode, 104 ... as the next door of insulating barrier, 104a ... form the peristome in region as film, 130 ... organic EL, 131 ... hole injection layer, 132 ... hole transporting layer, 133 ... luminescent layer, 136 ... functional layer, 140 ... as the print cartridge of ink reservoir, 1000 ... as the personal computer of electronic equipment, 1100 ... as the dull and stereotyped TV of electronic equipment.
Claims (19)
1. a functional layer formation ink, is characterized in that, contains:
The 1st composition that at least a kind of aromatic solvent that is 250 ℃～350 ℃ by boiling point forms,
Be 200 ℃ of the 2nd compositions that at least a kind of above aliphatic solvent forms by boiling point, and
Functional layer forms the 3rd composition of use;
For the dissolubility of described the 3rd composition, described the 1st composition is higher than described the 2nd composition,
The mixing ratio of described the 2nd composition is 30vol%～70vol%,
The boiling point of described the 1st composition is higher than the boiling point of described the 2nd composition, and the difference of the boiling point of the boiling point of described the 1st composition and described the 2nd composition is more than 30 ℃.
2. functional layer formation ink according to claim 1, is characterized in that, the surface tension of described the 2nd composition is less than described the 1st component list surface tension, and the surface tension of described the 2nd composition is below 32mN/m.
3. functional layer formation ink according to claim 2, is characterized in that, the n that described the 2nd composition is following chemical formulation is more than 2 fatty ether,
RO-(CH
2O)
n-R
Wherein, R is alkyl.
4. functional layer formation ink according to claim 3, is characterized in that, described the 2nd composition is selected from diethylene glycol butyl methyl ether or dibutyl ethylene glycol ether.
5. according to the functional layer formation ink described in any one in claim 1～4, it is characterized in that, described the 1st composition is to contain any the aromatic compound in nitrogen, oxygen, fluorine, chlorine at side chain.
6. functional layer formation ink according to claim 5, is characterized in that, described the 1st composition is selected from benzyl ether, 3-phenoxytoluene, 1, two (3, the 4-3,5-dimethylphenyl) ethane of 1-.
7. according to the functional layer formation ink described in any one in claim 1～6, it is characterized in that, described the 1st composition dissolves described the 3rd composition more than 0.1wt%.
8. according to the functional layer formation ink described in any one in claim 1～7, it is characterized in that, the mixed solvent of described the 1st composition and described the 2nd composition dissolves described the 3rd composition more than 0.1wt%.
9. according to the functional layer formation ink described in any one in claim 1～8, it is characterized in that, described the 1st composition contains multiple aromatic solvent.
10. according to the functional layer formation ink described in any one in claim 1～9, it is characterized in that, described the 3rd composition contains organic compound, and this organic compound is containing pi-conjugated macromolecular material or containing pi-conjugated low molecular material.
11. functional layer formation ink according to claim 10, is characterized in that, described the 3rd composition further contains metal complex.
12. according to the functional layer formation ink described in any one in claim 1～11, it is characterized in that, described the 3rd composition contains multiple organic compound.
13. 1 kinds of ink reservoirs, is characterized in that, the functional layer formation ink in the in-built requirement 1～12 of having the right described in any one.
14. 1 kinds of blowoffs, is characterized in that possessing:
Ink reservoir described in claim 13, and
Form the shower nozzle with ink from described ink reservoir functions of physical supply layer;
Described shower nozzle sprays described functional layer formation with drop form with ink from nozzle.
The formation method of 15. 1 kinds of functional layers, is characterized in that possessing:
Functional layer described in any one in claim 1～12 is formed to the operation that is coated on the film formation region of applied thing with ink, and
The described functional layer being coated with is formed and solidified with ink setting, form region and form the operation of functional layer at described film.
The formation method of 16. functional layers according to claim 15, is characterized in that, described film forms region and separated by the next door that described functional layer formation ink is had to liquid repellency.
The manufacture method of 17. 1 kinds of organic ELs, is characterized in that, is the manufacture method between anode and negative electrode with the organic EL of the functional layer that comprises luminescent layer, and the method possesses following operation:
Form the operation of separating the insulating barrier of described anode according to the mode overlapping with the outer rim of described anode and form peristome on described anode,
Functional layer in described peristome coating claim 10～12 described in any one forms the operation with ink,
The described functional layer being coated with is formed and solidified with ink setting, form the operation of at least 1 layer in described functional layer, and
Cover the operation that described insulating barrier and described functional layer form described negative electrode.
18. 1 kinds of light-emitting devices, is characterized in that, possess the organic EL that utilizes the manufacture method of the organic EL described in claim 17 to manufacture.
19. 1 kinds of electronic equipments, is characterized in that, possess the light-emitting device described in claim 18.
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| JP2012-252007 | 2012-11-16 | ||
| JP2012252007A JP6225413B2 (en) | 2012-11-16 | 2012-11-16 | Functional layer forming ink, ink container, ejection device, functional layer forming method, organic EL element manufacturing method |
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| CN103824959A true CN103824959A (en) | 2014-05-28 |
| CN103824959B CN103824959B (en) | 2018-08-31 |
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| CN201310566536.5A Active CN103824959B (en) | 2012-11-16 | 2013-11-14 | Functional layer is formed with ink, ink reservoir, blowoff, the forming method of functional layer, the manufacturing method of organic EL element, light-emitting device, electronic equipment |
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| Country | Link |
|---|---|
| US (1) | US10184056B2 (en) |
| JP (1) | JP6225413B2 (en) |
| KR (1) | KR102152271B1 (en) |
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Also Published As
| Publication number | Publication date |
|---|---|
| US20140138655A1 (en) | 2014-05-22 |
| TWI616499B (en) | 2018-03-01 |
| CN103824959B (en) | 2018-08-31 |
| KR20140066091A (en) | 2014-05-30 |
| US10184056B2 (en) | 2019-01-22 |
| TW201420702A (en) | 2014-06-01 |
| JP2014102878A (en) | 2014-06-05 |
| JP6225413B2 (en) | 2017-11-08 |
| KR102152271B1 (en) | 2020-09-04 |
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